BS ISO 2393-2014 Rubber test mixes Preparation mixing and vulcanization Equipment and procedures《橡胶试验胶料 配料 混炼和硫化 设备和程序》.pdf

1、BSI Standards PublicationBS ISO 2393:2014Rubber test mixes Preparation, mixing andvulcanization Equipmentand proceduresIncorporating corrigendum September 2015BS ISO 2393:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 2393:2014. Itsupersedes BS ISO 2393:2

2、008 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee PRI/22, Physical testing of rubber.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisi

3、ons of a contract. Users are responsible for its correctapplication. The British Standards Institution 2015. Published by BSI StandardsLimited 2015ISBN 978 0 580 91435 5ICS 83.060Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under

4、 the authority of theStandards Policy and Strategy Committee on 31 March 2014.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e d30 September 2015 Implementation of ISO corrected text 01 April2014: Numbering of subdivisions of subclausesamended, see ISO Foreword for details IS

5、O 2014Rubber test mixes Preparation, mixing and vulcanization Equipment and proceduresMlanges dessais base de caoutchouc Mlangeage, prparation et vulcanisation Appareillage et modes opratoiresINTERNATIONAL STANDARDISO2393Fourth edition2014-03-01Reference numberISO 2393:2014(E)Corrected version2014-0

6、4-01ISO 2393:2014(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 any form or by any means, electronic or mechanical, including photocopying, or posting on th

7、e 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 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb

8、 www.iso.orgPublished in SwitzerlandBS ISO 2393:2014ISO 2393:2014(E) ISO 2014 All rights reserved iiiContents PageForeword iv1 Scope . 12 Normative references 13 Terms and definitions . 14 Compounding ingredients 25 Preparation of materials 25.1 Batch masses 25.2 Weighing tolerances . 25.3 Carbon bl

9、ack conditioning 26 Mixing equipment . 26.1 Mixing mill 26.2 Laboratory internal mixer . 37 Mixing procedures 47.1 General . 47.2 Mill mixing procedure . 47.3 Laboratory internal mixer mixing procedure 58 Preparation of standard vulcanized sheets for dumb-bell test pieces . 78.1 Conditioning of batc

10、hes and blank preparation . 78.2 Vulcanization equipment . 88.3 Vulcanization procedure 109 Preparation of standard vulcanized discs for ring test pieces 119.1 Conditioning of batches and blank preparation 119.2 Vulcanization equipment 119.3 Vulcanization procedure 1210 Precision 12Annex A (informat

11、ive) Precision statement for both mill and internal mixer .14Annex B (informative) Internal mixer parameters and operating conditions for the three interlaboratory test programmes 21Annex C (informative) Further analysis of the ITP data 23Bibliography .24BS ISO 2393:2014ISO 2393:2014(E)ForewordISO (

12、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 technical commi

13、ttee 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 of electrotec

14、hnical 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 document was drafted

15、 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 patent right

16、s. 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 not constitu

17、te 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 informationThe commit

18、tee 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 fourth edition cancels and replaces the third edition (ISO 2393:2008), which has been technically revised: 7.1 has been added stating tha

19、t the Laboratory Internal Mixer is the preferred equipment; 7.2.1.1 has become 7.3.1.1; the subclause has been revised to delete the reference to EST8, which is no longer available, and because a control mix for a specific rubber type is not relevant in this International Standard; dimensions of the

20、 mould cavity have been specified in 8.2.2; instructions for removing trapped air after inserting the blanks have been added in 8.3.2.This corrected version of ISO 2393:2014 incorporates the following corrections: reinstatement of the numbering of subdivisions of subclauses 5.1, 5.2, 6.2, 7.2, 7.3.1

21、, 7.3.2, 7.3.3, 8.1, 8.3, 9.1.iv ISO 2014 All rights reservedBS ISO 2393:2014INTERNATIONAL STANDARD ISO 2393:2014(E)Rubber test mixes Preparation, mixing and vulcanization Equipment and procedures1 ScopeThis International Standard specifies the equipment and procedures for the preparation, mixing, a

22、nd vulcanization of rubber test mixes specified in the various International Standards for the evaluation of such test 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

23、, 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 289-1, Rubber, unvulcanized Determinations using a shearing-disc

24、 viscometer Part 1: Determination of Mooney viscosityISO 23529, Rubber General procedures for preparing and conditioning test pieces for physical test methods3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.3.1formulation batch massaggregate mass, i

25、n grams, of all the constituents in a formulation, with the rubber or oil-extended rubber polymer being taken as 100 g, or as specified in the appropriate evaluation procedure3.2batch massmass of test mix prepared in one mixing operation3.3total free volumevolume of the mixing chamber with the rotor

26、s in place3.4nominal mixer capacityproportion of the total free volume which is used in the mixing processNote 1 to entry: A value of 0,75 times the total free volume has been found suitable for mixers with tangential rotors.3.5evaluation procedureInternational Standard specifying the materials, tes

27、t formulation, mixing procedure, vulcanization procedure, and test methods for the evaluation of a type of rubber or compounding ingredient ISO 2014 All rights reserved 1BS ISO 2393:2014ISO 2393:2014(E)4 Compounding ingredientsThe compounding ingredients required for the various standard test formul

28、ations shall be in accordance with National or International Standards as specified in the appropriate evaluation procedure.5 Preparation of materials5.1 Batch masses5.1.1 The standard batch mass for the laboratory mill, in grams, shall be four times the formulation batch mass unless otherwise state

29、d in the appropriate evaluation procedure.NOTE Smaller batch masses are used in some countries. These may not give identical results.5.1.2 The batch mass for the laboratory internal mixer, in grams, shall be equal to the nominal mixer capacity, in cubic centimetres, multiplied by the compound densit

30、y.5.2 Weighing tolerances5.2.1 The batch mass shall be taken into consideration when determining weighing tolerances. In general, rubber and carbon black shall be weighed to the nearest 1 g, oil to the nearest 1 g or 1 %, whichever is the more accurate, vulcanizing agents and accelerators to the nea

31、rest 0,02 g and zinc oxide and stearic acid to the nearest 0,1 g. All other ingredients shall be weighed to an accuracy of 1 %.5.2.2 When the batch mass is less than four times the formulation batch mass, the weighing tolerances shall be one tenth of those given in 5.2.1. Therefore, the rubber and c

32、arbon black shall be weighed to the nearest 0,1 g, oil to the nearest 0,1 g or 1 % whichever is the more accurate, sulfur and accelerators to the nearest 0,002 g and zinc oxide and stearic acid to the nearest 0,01 g. All other ingredients shall be weighed to an accuracy of 1 %.5.3 Carbon black condi

33、tioningUnless otherwise specified, carbon black shall be conditioned, before weighing, by heating in an oven at a temperature of 105 C 5 C for 2 h. The black shall be placed in an open vessel of suitable dimensions, so that the depth of the black is no more than 10 mm during conditioning. The black,

34、 conditioned as above, shall be stored in a closed moisture-proof container until it is required for mixing.Alternatively, carbon black may be conditioned by heating in an oven at 125 C 3 C for 1 h. Carbon black conditioned in this manner may not give the same results as that conditioned at 105 C 5

35、C.The conditioning temperature used shall be recorded in the batch-mixing report.6 Mixing equipment6.1 Mixing millThe characteristics of a standard laboratory mill are as follows: roll diameter (OD) 150 mm to 155 mm; roll length (between guides) 250 mm to 280 mm; speed of front (slow) roll 24 r/min

36、1 r/min; roll-speed ratio preferably 1:1,4; clearance between rolls (adjustable) 0,2 mm to 8,0 mm;2 ISO 2014 All rights reservedBS ISO 2393:2014ISO 2393:2014(E) temperature-control tolerance 5 C (unless otherwise specified).WARNING The mill should be equipped with suitable safety devices to protect

37、against accidents and the operator should be provided with suitable equipment to protect against hazardous chemicals, in accordance with national safety regulations.NOTE 1 If mills of other dimensions are used, adjustments to batch masses and mixing cycles may be required to obtain comparable result

38、s.NOTE 2 If the roll-speed ratio is other than 1:1,4, modifications may be necessary to the mixing procedure to obtain comparable results.The roll clearance shall be determined by means of two lead strips 10 mm 3 mm in width, at least 50 mm long and 0,25 mm to 0,50 mm thicker than the roll clearance

39、 to be measured. The lead strips shall be inserted, one at each end of the rolls, approximately 25 mm from the guides, while a piece of compounded rubber with a Mooney viscosity, determined in accordance with ISO 289-1, greater than 50 ML(1+4) at 100 C and measuring approximately 75 mm 75 mm 6 mm is

40、 passing through the centre portion of the nip. The rolls shall be at the temperature specified for mixing. After passing between the rolls, the thickness of the lead strips shall be measured at three separate positions with a micrometer to an accuracy of 0,01 mm. The tolerance on roll clearance sha

41、ll be 10 % or 0,05 mm, whichever is the larger.The mill rolls shall have provision for circulation of heating or cooling media.6.2 Laboratory internal mixer6.2.1 Laboratory internal mixers are available in a variety of sizes ranging from a nominal mixer capacity of 65 cm3(described previously as a m

42、iniature internal mixer) to about 3 000 cm3. Interlaboratory test programmes (ITPs) on two different types of synthetic rubber and on natural rubber have shown that mixer capacity does not have a significant effect on the results, provided that good dispersion of all ingredients is achieved (see Ann

43、ex C for a discussion of the effects of certain mixer variables).For interlaboratory comparisons, it is preferable to use the same type of mixer and to align the mixing conditions (nominal mixing capacity, mixer head starting temperature, rotor type, and speed, mixing time) as closely as possible.Al

44、l of the mixers used in the interlaboratory test programmes (ITPs) were of the tangential-rotor type, and included Banbury, cam, and other types. No laboratory suggested using an intermeshing-rotor mixer. Therefore, the mixer described as type B in the previous edition of this International Standard

45、 has been deleted. However, an intermeshing type may be used when the interested parties agree.6.2.2 This International Standard describes general requirements for laboratory internal mixers ranging in nominal mixer capacity from about 65 cm3to about 2 000 cm3.WARNING Laboratory internal mixers shou

46、ld be equipped with a suitable exhaust system and suitable safety devices to prevent accidents, in accordance with national safety regulations. The operators should be provided with suitable equipment to protect them against hazardous chemicals, in accordance with national regulations.NOTE The small

47、er laboratory internal mixers can only provide enough compound for curemeter testing and limited stress-strain testing.6.2.3 All laboratory internal mixers shall be fitted with a system to measure and indicate and/or record the temperature of the mix during the mixing operation to within 1 C.NOTE Th

48、e actual mix temperature usually exceeds the indicated temperatures by an amount dependent on the mixing conditions used and the location of the measuring probe.6.2.4 All laboratory internal mixers shall be fitted with a timer to indicate the mixing time to 5 s. ISO 2014 All rights reserved 3BS ISO

49、2393:2014ISO 2393:2014(E)6.2.5 All laboratory internal mixers shall be fitted with a system to indicate or record electrical power demand or torque.6.2.6 All laboratory internal mixers shall be fitted with an efficient heating and cooling system to control the surface temperature of the rotors and the mixing-chamber walls.6.2.7 All laboratory internal mixers shall be closed during the mixing cycle with a ram to contain the mix in the mixing chamber.6.2.8 When rotor clearances exceed the