1、BSI Standards Publication BS ISO 7663:2014 Halogenated isobutene- isoprene rubber (BIIR and CIIR) Evaluation proceduresBS ISO 7663:2014 BRITISH STANDARD National foreword This British Standard is the UK implementation of ISO 7663:2014. It supersedes BS ISO 7663:2005 which is withdrawn. The UK partic
2、ipation in its preparation was entrusted to Technical Committee PRI/50, Rubber - Raw, natural and synthetic, including latex and carbon black. 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 neces
3、sary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2014. Published by BSI Standards Limited 2014 ISBN 978 0 580 85479 8 ICS 83.060 Compliance with a British Standard cannot confer immunity from legal obligations. This British Standard
4、was published under the authority of the Standards Policy and Strategy Committee on 30 September 2014. Amendments issued since publication Date Text affectedBS ISO 7663:2014 ISO 2014 Halogenated isobutene-isoprene rubber (BIIR and CIIR) Evaluation procedures Caoutchoucs isobutne-isoprne halogns (BII
5、R et CIIR) Mthodes dvaluation INTERNATIONAL STANDARD ISO 7663 Fifth edition 2014-10-01 Reference number ISO 7663:2014(E)BS ISO 7663:2014ISO 7663:2014(E)ii ISO 2014 All rights reserved COPYRIGHT PROTECTED DOCUMENT ISO 2014 All rights reserved. Unless otherwise specified, no part of this publication m
6、ay 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 permission. Permission can be requested from either ISO at the address below or ISOs member body in the country of th
7、e requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in SwitzerlandBS ISO 7663:2014ISO 7663:2014(E) ISO 2014 All rights reserved iii Contents Page Foreword iv 1 Scope . 1 2 Normative referen
8、ces 1 3 Sampling and further preparative procedures . 1 4 Physical and chemical tests on raw rubber 2 4.1 Mooney viscosity . 2 4.2 Volatile matter . 2 4.3 Ash . 2 5 Preparation of test mixes. 2 5.1 Standard test formulation . 2 5.2 Procedure 2 6 Evaluation of vulcanization characteristics by a curem
9、eter test . 5 6.1 Using an oscillating-disc curemeter 5 6.2 Using a rotorless curemeter 5 7 Evaluation of tensile stress-strain properties of vulcanized test mixes .5 8 Precision . 5 9 Test report . 6 Annex A (informative) Precision . 7 Bibliography 9BS ISO 7663:2014ISO 7663:2014(E) Foreword ISO (th
10、e 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 committ
11、ee 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 electrotechn
12、ical 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
13、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 rights
14、. 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 constitut
15、e 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 information The commi
16、ttee 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 fifth edition cancels and replaces the fourth edition (ISO 7663:2005), which has been technically revised with the following changes: C
17、lause 2 has been updated; in 4.2, the method given in ISO 248-2 is now allowed; in 5.2.2.1, addition of a statement that the mixing with a laboratory internal mixer is the preferred procedure. Method B becomes “Single stage mixing with a laboratory internal mixer”; in 5.2.2.3, advice on mixing with
18、various sizes of laboratory internal mixer is given along with a general mixing procedure.iv ISO 2014 All rights reservedBS ISO 7663:2014INTERNATIONAL ST ANDARD ISO 7663:2014(E) Halogenated isobutene-isoprene rubber (BIIR and CIIR) Evaluation procedures WARNING Persons using this International Stand
19、ard 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 ensure compliance with any nat
20、ional regulatory conditions. 1 Scope This International Standard specifies the following: physical and chemical tests on raw rubbers; standardized materials, a standardized test formulation, and the equipment and processing methods for evaluating the vulcanization characteristics of all types of hal
21、ogenated isobutene- isoprene rubber (BIIR and CIIR). 2 Normative references The 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, the latest ed
22、ition of the referenced document (including any amendments) applies. ISO 37, Rubber, vulcanized or thermoplastic Determination of tensile stress-strain properties ISO 247, Rubber Determination of ash ISO 248-1, Rubber, raw Determination of volatile-matter content Part 1: Hot-mill method and oven met
23、hod ISO 248-2, Rubber, raw Determination of volatile-matter content Part 2: Thermogravimetric methods using an automatic analyser with an infrared drying unit ISO 289-1, Rubber, unvulcanized Determinations using a shearing-disc viscometer Part 1: Determination of Mooney viscosity ISO 1795:2007, Rubb
24、er, raw natural and raw synthetic Sampling and further preparative procedures ISO 2393, Rubber test mixes Preparation, mixing and vulcanization Equipment and procedures ISO 3417, Rubber Measurement of vulcanization characteristics with the oscillating disc curemeter ISO 6502, Rubber Guide to the use
25、 of curemeters ISO 23529, Rubber General procedures for preparing and conditioning test pieces for physical test methods 3 Sampling and further preparative procedures 3.1 Selection of the sample from the lot shall be in accordance with ISO 1795. 3.2 Take a laboratory sample of approximately 1,5 kg b
26、y the method described in ISO 1795. 3.3 Prepare test samples in accordance with ISO 1795. ISO 2014 All rights reserved 1BS ISO 7663:2014ISO 7663:2014(E) 4 Physical and chemical tests on raw rubber 4.1 Mooney viscosity Prepare a test sample, without milling, in accordance with the preferred procedure
27、 in ISO 1795. If milling is deemed necessary, either because of the condition of the laboratory sample (e.g. excessive porosity) or by agreement between the interested parties, it shall be performed in accordance with ISO 1795:2007, 7.3.2.2, paragraphs 1 and 2. Determine the Mooney viscosity in acco
28、rdance with ISO 289-1 on a test piece cut from the test sample which shall be as free as possible from air and pockets that may trap air against the rotor and die surface. The viscosity shall be determined as ML(1+8) at 125 C. 4.2 Volatile matter Determine the volatile-matter content by the hot-mill
29、 method as specified in ISO 248-1 or by the method specified in ISO 248-2. 4.3 Ash Determine the ash in accordance with either method A or method B of ISO 247. 5 Preparation of test mixes 5.1 Standard test formulation The standard test formulation is given in Table 1. The materials shall be national
30、 or international standard reference materials. If no standard reference material is available, the materials to be used shall be agreed by the parties concerned. Table 1 Standard test formulation for evaluation of halogenated isobutene-isoprene rubbers Material Parts by mass Halogenated isobutene-i
31、soprene rubber (BIIR or CIIR) 100,00 Stearic acid a, b 1,00 Industry reference black c 40,00 Zinc oxide a, d 5,00 Tot al 146,00 aUse powder materials. bThe standard reference material for stearic acid is specified in ISO 8312. Use class A. cUse the current industry reference black. dThe standard ref
32、erence material for zinc oxide is specified in ISO 9298. Use the indirect (French) process. 5.2 Procedure 5.2.1 Equipment and procedure The equipment and procedure for the preparation, mixing and vulcanization shall be in accordance with ISO 2393.2 ISO 2014 All rights reservedBS ISO 7663:2014ISO 766
33、3:2014(E) 5.2.2 Mixing procedure 5.2.2.1 General Two alternative mixing procedures are specified, but in accordance with ISO 2393 the laboratory internal mixer procedure is preferred: method A: mill mixing; method B: single stage mixing with a laboratory internal mixer. NOTE The above procedures may
34、 not give identical results. 5.2.2.2 Method A (mill mixing procedure) The standard laboratory mill batch mass, in grams, shall be based on four times the formulation mass, i.e. 4 146,00 g (= 584 g). The surface temperatures of the rolls shall be maintained at 40 C 5 C throughout the mixing. The vulc
35、anization of halogenated isobutene-isoprene rubber with zinc oxide is highly sensitive to moisture. Therefore, care shall be taken when conditioning the carbon black. Condition the carbon black for 1 h at 125 C 3 C. The thickness of the carbon black layer shall not exceed 10 mm. Store the conditione
36、d black in a moisture-proof container. Maintain a good rolling bank at the nip of the rolls during mixing. If this is not obtained with the nip settings specified below, small adjustments to the mill openings can be necessary. Mix the stearic acid and the carbon black together in a suitable containe
37、r before starting to mix. Duration (min) Cumulative time (min) a) Band the rubber on the slow roll with the mill opening set at 0,65 mm 1,0 1,0 b) Add the mixture of stearic acid and carbon black evenly across the mill at a uniform rate. Return any materials that drop through the mill to the batch.
38、9,5 10,5 c) When all the mixture of stearic acid and carbon black has been incorpo- rated, make one 3/4 cut from each side. Do not cut the band until all visible free black has been incorporated. 0,5 11,0 d) Add the zinc oxide. 3,0 14,0 e) When all the zinc oxide has been incorporated, make three 3/
39、4 cuts from each side, alternately. 2,0 16,0 f) Cut the batch from the mill. Set the mill opening at 0,8 mm and pass the rolled batch endwise through the mill six times. 2,0 18,0 g) Sheet the batch to a thickness of approximately 6 mm. Check-weigh the batch (see ISO 2393). If the mass of the batch d
40、iffers from the theoretical value by more than +0,5 %/1,5 %, discard the batch and re-mix. h) Sheet the batch to a thickness of approximately 2,2 mm for preparing test sheets or to the appro- priate thickness for preparing ISO ring test pieces in accordance with ISO 37. i) Condition the batch for 2
41、h to 24 h prior to vulcanizing and curemeter testing at standard labora- tory temperature and humidity as defined in ISO 23529. ISO 2014 All rights reserved 3BS ISO 7663:2014ISO 7663:2014(E) 5.2.2.3 Method B (single stage mixing with a laboratory internal mixer procedure) For laboratory internal mix
42、ers having nominal capacities of 65 cm 3to about 2 000 cm 3 , the batch mass shall be equal to the nominal mixer capacity, in cubic centimetres, multiplied by the density of the compound. For each batch mixed, the laboratory internal mixer conditions shall be the same during the preparation of a ser
43、ies of identical mixes. 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 laboratory internal mixer shall be allowed to cool down to 60 C between the end of one test batch and the start of the next. The
44、 temperature control conditions shall not be altered during the mixing of a series of test batches. The mixing technique shall be such as to obtain a good dispersion of all the ingredients. Condition the carbon black as described in 5.2.2.2. NOTE A general mixing procedure for the laboratory interna
45、l mixer is as follows: Duration (min) Cumulative time (min) a) Charge the stearic acid, zinc oxide, and carbon black first, followed by 3/4 of the rubber, lower the ram and start the timer. 0,0 0,0 b) Allow the batch to mix, raise the ram to sweep down, if necessary. Add the rest of the rubber. 1,5
46、1,5 c) Allow the batch to mix. 3,5 5,0 d) Turn off the rotor, raise the ram, open the mixing chamber, and discharge the batch. Record the maximum batch temperature. The final temperature of the batch discharged after 5 min shall not exceed 120 C. If necessary, adjust the batch mass or the head tempe
47、rature so that this condition is achieved. e) Immediately pass the batch twice through a mill set at 40 C 5 C with a mill opening of 3,0 mm or compress the batch between two stainless-steel plates with a force of 100 kN for 5 s at 30 C 5 C. f) Check-weigh the batch (see ISO 2393). If the mass of the
48、 batch differs from the theoretical value by more than +0,5 %/1,5 %, discard the batch and remix. g) Condition the batch for 2 h to 24 h at standard laboratory temperature and humidity as defined in ISO 23529. Cut a test piece for curemeter testing in accordance with either 6.1 or 6.2. h) If require
49、d, sheet the batch to approximately 2,2 mm for preparing test sheets or to the appropri- ate thickness for preparing ring test pieces in accordance with ISO 37. Condition the batch in accord- ance with g) above. For a laboratory internal mixer having a nominal capacity of 65 cm 3a batch mass corresponding to 0,48 times the formulation mass, i.e. 0,48 146,00 (= 70,08 g) has been found to be suitable. Prepare the rubber by passing it once through a mill with the temperature se
