1、BSI Standards PublicationBS ISO 7663:2014Halogenated isobutene-isoprene rubber (BIIR and CIIR) Evaluation proceduresBS ISO 7663:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 7663:2014. Itsupersedes BS ISO 7663:2005 which is withdrawn.The UK participation
2、 in its preparation 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 necessaryprovisio
3、ns of a contract. Users are responsible for its correctapplication. The British Standards Institution 2014. Published by BSI StandardsLimited 2014ISBN 978 0 580 85479 8ICS 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 30 September 2014.Amendments issued since publicationDate Text affectedBS ISO 7663:2014 ISO 2014Halogenated isobutene-isoprene rubber (BIIR and CIIR) Evaluation proceduresCaoutchoucs isobutne-isoprne halogns (BIIR et CIIR) Mthodes dvalua
5、tionINTERNATIONAL STANDARDISO7663Fifth edition2014-10-01Reference numberISO 7663:2014(E)BS ISO 7663:2014ISO 7663:2014(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 other
6、wise 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 the requester.ISO copyright officeCa
7、se postale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 7663:2014ISO 7663:2014(E) ISO 2014 All rights reserved iiiContents PageForeword iv1 Scope . 12 Normative references 13 Sampling and further preparative proce
8、dures . 14 Physical and chemical tests on raw rubber 24.1 Mooney viscosity . 24.2 Volatile matter . 24.3 Ash . 25 Preparation of test mixes. 25.1 Standard test formulation . 25.2 Procedure 26 Evaluation of vulcanization characteristics by a curemeter test . 56.1 Using an oscillating-disc curemeter 5
9、6.2 Using a rotorless curemeter 57 Evaluation of tensile stress-strain properties of vulcanized test mixes . 58 Precision . 59 Test report . 6Annex A (informative) Precision . 7Bibliography 9BS ISO 7663:2014ISO 7663:2014(E)ForewordISO (the International Organization for Standardization) is a worldwi
10、de 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 committee has been established has the right to be represented on tha
11、t 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 electrotechnical standardization.The procedures used to develop this docum
12、ent 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 in accordance with the editorial rules of the ISO/IEC Directive
13、s, 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. Details of any patent rights identified during the developmen
14、t 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 constitute an endorsement.For an explanation on the meaning of ISO speci
15、fic 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 committee responsible for this document is ISO/TC 45, Rubber and rubbe
16、r 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: Clause 2 has been updated; in 4.2, the method given in ISO 248-2 is
17、 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 various sizes of laboratory internal mixer is given along with a g
18、eneral mixing procedure.iv ISO 2014 All rights reservedBS ISO 7663:2014INTERNATIONAL STANDARD ISO 7663:2014(E)Halogenated isobutene-isoprene rubber (BIIR and CIIR) Evaluation proceduresWARNING Persons using this International Standard should be familiar with normal laboratory practice. This Internat
19、ional 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 national regulatory conditions.1 ScopeThis International Standard specif
20、ies 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 halogenated isobutene-isoprene rubber (BIIR and CIIR).2 Normative referenc
21、esThe 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 edition of the referenced document (including any amendments) applies.ISO 37
22、, 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 oven methodISO 248-2, Rubber, raw Determination of volatile-matter content Part 2: Th
23、ermogravimetric methods using an automatic analyser with an infrared drying unitISO 289-1, Rubber, unvulcanized Determinations using a shearing-disc viscometer Part 1: Determination of Mooney viscosityISO 1795:2007, Rubber, raw natural and raw synthetic Sampling and further preparative proceduresISO
24、 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 curemetersISO 23529, Rubber General procedures for preparing and conditioning t
25、est pieces for physical test methods3 Sampling and further preparative procedures3.1 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 by the method described in ISO 1795.3.3 Prepare test samples in accordance with ISO 1795
26、. ISO 2014 All rights reserved 1BS ISO 7663:2014ISO 7663:2014(E)4 Physical and chemical tests on raw rubber4.1 Mooney viscosityPrepare a test sample, without milling, in accordance with the preferred procedure in ISO 1795.If milling is deemed necessary, either because of the condition of the laborat
27、ory 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 accordance with ISO 289-1 on a test piece cut from the test sample which shall be as free as poss
28、ible 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 matterDetermine the volatile-matter content by the hot-mill method as specified in ISO 248-1 or by the method specified in ISO 248-2.4.3 AshDetermine the a
29、sh in accordance with either method A or method B of ISO 247.5 Preparation of test mixes5.1 Standard test formulationThe standard test formulation is given in Table 1. The materials shall be national or international standard reference materials. If no standard reference material is available, the m
30、aterials to be used shall be agreed by the parties concerned.Table 1 Standard test formulation for evaluation of halogenated isobutene-isoprene rubbersMaterial Parts by massHalogenated isobutene-isoprene rubber (BIIR or CIIR) 100,00Stearic acida, b1,00Industry reference blackc40,00Zinc oxidea, d5,00
31、Total 146,00aUse 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 reference material for zinc oxide is specified in ISO 9298. Use the indirect (French) process.5.2 Procedure5.2.1 Equipment
32、 and procedureThe 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 7663:2014(E)5.2.2 Mixing procedure5.2.2.1 GeneralTwo alternative mixing procedures are specified, but in accordance with ISO
33、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 not give identical results.5.2.2.2 Method A (mill mixing procedure)The standard laboratory mill batch mass, in grams, shall b
34、e 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 vulcanization of halogenated isobutene-isoprene rubber with zinc oxide is highly sensitive to moisture. Therefore, care shall be take
35、n 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 conditioned black in a moisture-proof container.Maintain a good rolling bank at the nip of the rolls during mixing. If this is not obtained
36、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 container 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
37、 1,0 1,0b) 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.9,5 10,5c) 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 b
38、and until all visible free black has been incorporated.0,5 11,0d) Add the zinc oxide. 3,0 14,0e) When all the zinc oxide has been incorporated, make three 3/4 cuts from each side, alternately.2,0 16,0f) Cut the batch from the mill. Set the mill opening at 0,8 mm and pass the rolled batch endwise thr
39、ough the mill six times.2,0 18,0g) Sheet the batch to a thickness of approximately 6 mm. Check-weigh the batch (see ISO 2393). If the mass of the batch differs 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
40、 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 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 res
41、erved 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 mixers having nominal capacities of 65 cm3to about 2 000 cm3, the batch mass shall be equal to the nominal mixer capacity, in cubic centimetres, multiplied
42、by the density of the compound. For each batch mixed, the laboratory internal mixer conditions shall be the same during the preparation of a series 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 u
43、nder 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 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 dis
44、persion of all the ingredients.Condition the carbon black as described in 5.2.2.2.NOTE A general mixing procedure for the laboratory internal 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 th
45、e ram and start the timer.0,0 0,0b) Allow the batch to mix, raise the ram to sweep down, if necessary. Add the rest of the rubber.1,5 1,5c) Allow the batch to mix. 3,5 5,0d) Turn off the rotor, raise the ram, open the mixing chamber, and discharge the batch. Record the maximum batch temperature.The
46、final temperature of the batch discharged after 5 min shall not exceed 120 C. If necessary, adjust the batch mass or the head temperature 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
47、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 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
48、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 required, 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
49、 batch in accord-ance with g) above.For a laboratory internal mixer having a nominal capacity of 65 cm3a 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 set at 50 C 5 C and an opening of 0,5 mm. Cut the sheet into 20 mm wide strips.Mix with the head temperature maintained at 60 C 3 C and the unloaded rotor speed at 6,3
