1、BSI Standards PublicationBS ISO 4097:2014Rubber, ethylene-propylene-diene (EPDM) EvaluationprocedureBS ISO 4097:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 4097:2014. Itsupersedes BS ISO 4097:2007 which is withdrawn.The UK participation in its preparat
2、ion was entrusted to TechnicalCommittee PRI/50, Rubber - Raw, natural and synthetic, includinglatex and carbon black.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract
3、. Users are responsible for its correctapplication. The British Standards Institution 2014. Published by BSI StandardsLimited 2014ISBN 978 0 580 77199 6ICS 83.060Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of
4、 theStandards Policy and Strategy Committee on 30 September 2014.Amendments issued since publicationDate Text affectedBS ISO 4097:2014 ISO 2014Rubber, ethylene-propylene-diene (EPDM) Evaluation procedureCaoutchouc thylne-propylne-dine (EPDM) Mthode dvaluationINTERNATIONAL STANDARDISO4097Sixth editio
5、n2014-10-01Reference numberISO 4097:2014(E)BS ISO 4097:2014ISO 4097:2014(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
6、or mechanical, including photocopying, or 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 officeCase postale 56 CH-1211 Geneva 20Tel. + 41 22 7
7、49 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 4097:2014ISO 4097:2014(E) ISO 2014 All rights reserved iiiContents PageForeword iv1 Scope . 12 Normative references 13 Sampling and sample preparation 14 Physical and chemical tests on raw rubber 24.1 M
8、ooney viscosity . 24.2 Volatile matter . 24.3 Ash . 25 Preparation of test mixes for evaluation . 25.1 Standard test formulations . 25.2 Equipment and procedure 35.3 Mixing procedures . 36 Evaluation of vulcanization characteristics by a curemeter test . 86.1 Using an oscillating-disc curemeter 86.2
9、 Using a rotorless curemeter 87 Evaluation of tensile stress-strain properties of vulcanized test mixes . 98 Precision . 99 Test report . 9Annex A (informative) Precision 10Annex B (informative) Standard test formulations of ISO 4097:2007 .13Bibliography .16BS ISO 4097:2014ISO 4097:2014(E)ForewordIS
10、O (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 co
11、mmittee 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 electro
12、technical 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 draf
13、ted 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 ri
14、ghts. 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 const
15、itute 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 com
16、mittee 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 4097:2007), which has been technically revised with the following changes: a
17、ddition of new standard test formulations for the evaluation of EPDM rubbers (Table 1); removal of tetramethyl thiuram disulfide (TMTD) from the standard test formulations; changes in mixing procedures (5.3): inclusion of two-stage mixing and laboratory internal mixer; addition of a statement that s
18、ingle-stage mixing is the preferred method (5.3.1); addition of new precision data in a new informative Annex A; the standard test formulations and the precision data of the fifth edition (ISO 4097:2007) were moved to a new informative Annex B; addition of a statement in Annex B to explain that the
19、standard formulations of the fifth edition (ISO 4097:2007) are retained until the next systematic review with a limitation of five years.iv ISO 2014 All rights reservedBS ISO 4097:2014INTERNATIONAL STANDARD ISO 4097:2014(E)Rubber, ethylene-propylene-diene (EPDM) Evaluation procedureWARNING Persons u
20、sing 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 practices and to e
21、nsure 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 for evaluating the vulcanization characteristics of ethyl
22、ene-propylene-diene rubbers (EPDM), including oil-extended types.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, only the edition cited applies. For undated references, th
23、e 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, raw Determination of volatile-matter content Part 1: Hot-mill method and
24、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, unvulcanised Determinations using a shearing-disc viscometer Part 1: Determination of Mooney viscosityISO 1795, Rubb
25、er, 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 characteristics with the oscillating disc curemeterISO 6502, Rubber Guide to the use of
26、 curemetersISO 23529, Rubber General procedures for preparing and conditioning test pieces for physical test methods3 Sampling and sample preparation3.1 Take a laboratory sample of approximately 1,5 kg by the method described in ISO 1795.3.2 Prepare the test portion in accordance with ISO 1795. ISO
27、2014 All rights reserved 1BS ISO 4097:2014ISO 4097:2014(E)4 Physical and chemical tests on raw rubber4.1 Mooney viscosityDetermine the Mooney viscosity in accordance with ISO 289-1, on a test portion prepared as indicated in 3.2 (without massing).If massing is necessary, maintain the mill roll surfa
28、ce temperature at 50 C 5 C (for rubbers with a low Mooney viscosity, a temperature of 35 C 5 C can be used). Massing, if used, shall be mentioned in the test report.Record the result as ML(1+4) at 125 C unless another test temperature (100 C or 150 C) and/or test time (1+8) min has been agreed by th
29、e interested parties.4.2 Volatile matterDetermine the volatile matter content in accordance with ISO 248-1 or ISO 248-2.4.3 AshDetermine the ash content in accordance with method A or method B of ISO 247.5 Preparation of test mixes for evaluation5.1 Standard test formulationsThe standard test formul
30、ations are given in Table 1, in which:a) formulation 1 is applicable to non-oil-extended EPDMs with a nominal ethylene content not higher than 67 % by mass;b) formulation 2 is applicable to non-oil-extended EPDMs with a nominal ethylene content equal to or higher than 67 % by mass;c) formulation 3 i
31、s applicable to non-oil-extended low Mooney viscosity EPDMs;d) formulation 4 is applicable to oil-extended EPDMs containing 50 or less parts by mass of oil per 100 parts of rubber;e) formulation 5 is applicable to oil-extended EPDMs containing more than 50 but less than 80 parts by mass of oil per 1
32、00 parts of rubber;f) formulation 6 is applicable to oil-extended EPDMs containing 80 or more parts by mass of oil per 100 parts of rubber.The materials used shall be national or International Standard reference materials unless no standard reference material is available in which case the materials
33、 to be used shall be agreed between the interested parties.2 ISO 2014 All rights reservedBS ISO 4097:2014ISO 4097:2014(E)Table 1 Standard test formulations for evaluation of EPDM rubbersMaterialTest formulation 1 2 3 4 5 6Parts by massEPDM 100,00 100,00 100,00 100,00 + xa100,00 + yb100,00 + zcSteari
34、c acid 1,00 1,00 1,00 1,00 1,00 1,00Industry reference blackd80,00 100,00 40,00 80,00 80,00 150,00ASTM 103 oile50,00 75,00 50,00 xa Zinc oxide 5,00 5,00 5,00 5,00 5,00 5,00Sulfur 1,50 1,50 1,50 1,50 1,50 1,50N-Cyclohexyl-2-Mercaptobenzothiazilesulphenamide(CBS)3,5 3,5 3,5 3,5 3,5 3,5Mercaptobenzothi
35、azole (MBT)1,0 1,0 1,0 1,0 1,0 1,0Total 242,00 287,00 152,00 242,00 192,00 + yb262,00 + zcax is the number of parts by mass of oil per 100 parts of base rubber for types having an oil content of 50 or less.by is the number of parts by mass of oil per 100 parts of base rubber for types having an oil
36、content more than 50 but less than 80.cz is the number of parts by mass of oil per 100 parts of base rubber for types having a minimum oil content of 80.dThe current industry reference black (IRB) is used.eThis oil density is 0,92 g/cm3. Alternative oils can be used but might give slightly different
37、 results. ASTM 103 oil is an example of a suitable product available commercially. It is produced by the Sun Refining and Marketing Company and distributed by R.E. Carroll Inc., 1570 North Olden Avenue Ext, Trenton, NJ 08638, USA. Overseas requests should be directed to Sunoco Overseas Inc., 1801 Ma
38、rket Street, Philadelphia, PA 19103-1699, USA. This information is given for the convenience of users of this International Standard and does not constitute an endorsement by ISO of this product.5.2 Equipment and procedureEquipment and procedure for the preparation, mixing, and vulcanization shall b
39、e in accordance with ISO 2393.5.3 Mixing procedures5.3.1 GeneralFour alternative mixing procedures are specified. Method A1: single stage mixing with LIM (laboratory internal mixer) which is the preferred method. Method A2: two-stage mixing with LIM. Method A3: two-stage mixing using a LIM for initi
40、al mixing and mill mixing for final mixing. Method B: mill mixing.Mixing of ethylene-propylene-diene rubbers in the standard test formulations using a mill is more difficult than for other rubbers and the use of a LIM allows better results. Because of the difficulty of mill mixing EPDM rubbers, it i
41、s recommended that method B be used only if a LIM is not available. ISO 2014 All rights reserved 3BS ISO 4097:2014ISO 4097:2014(E)5.3.2 LIM mixing for methods A1, A2, and A35.3.2.1 GeneralThe mixing technique in each method can be modified to achieve a good dispersion of all the ingredients. The LIM
42、 conditions shall be the same during the preparation of a series of identical mixes for each batch mixed. 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 LIM shall be allowed to cool down to 60 C betwe
43、en the end of one test batch and the start of the next. Temperature control condition shall not be altered during the mixing of a series of test.5.3.2.2 Method A1 Single stage mixing with LIMThe final temperature of the batch discharged after mixing shall not exceed 120 C. If necessary, adjust the b
44、atch mass, head temperature, or rotors speed, so that this condition is met.Compounding materials other than rubber, carbon black, and oil can be added to LIM batches more precisely and with greater ease if they are previously blended together in the proportions required by the formulation. Such ble
45、nds can be made using a mortar and pestle, by mixing for 10 min in a biconical blender with intensifier bar turning, or by mixing in a blender for five 3 s-periods and scraping the inside of the blender to dislodge materials stuck to the sides after each 3 s-mix. A Waring1)blender has been found sui
46、table for this method.Caution If mixed longer than 3 s, the stearic acid can melt and prevent good dispersion.NOTE An example of mixing procedure for LIM is as follows.Duration (min) Cumulative time (min) a) Load the rubber, lower the ram and allow the rubber to be masti-cated. 1,0 1,0 b) Raise the
47、ram and add the pre-blended zinc oxide, sulfur, stearic acid, and accelerators, taking care to avoid any loss. Then add the car-bon black and oil, sweep the orifice, and lower the ram. 1,0 2,0 c) Allow the batch to mix. 7,0 _9,0 Total time (max) 9,0 d) Turn off the motor, raise the ram, remove the m
48、ixing chamber, and discharge the batch. Record the maximum batch temperature.e) After discharging the mixed batch, immediately pass it through a laboratory mill with its mill opening set at 0,8 mm and at a temperature of 50 C 5 C.f) Pass the rolled batch endwise through the rolls six times.g) Sheet
49、the batch to approximately 6 mm. Check-weigh the batch (see ISO 2393). If the mass of the batch differs from the theoretical value by more than 1,5 % to +0,5 %, discard the batch and re-mix.h) Remove sufficient material for cure testing.i) Sheet the batch to approximately 2,2 mm for preparing test sheets or to the appropriate thickness for preparing ISO ring test pieces in accordance with ISO 37.1) This information is given for the convenience of users of this Int
