1、BSI Standards PublicationBS ISO 2322:2014Styrene-butadiene rubber(SBR) Emulsion- andsolution-polymerized types Evaluation proceduresBS ISO 2322:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 2322:2014. Itsupersedes BS ISO 2322:2009 which is withdrawn.The
2、UK participation 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 n
3、ecessaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2014. Published by BSI StandardsLimited 2014ISBN 978 0 580 79383 7ICS 83.060Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was
4、published under the authority of theStandards Policy and Strategy Committee on 28 February 2014.Amendments issued since publicationDate Text affectedBS ISO 2322:2014 ISO 2014Styrene-butadiene rubber (SBR) Emulsion- and solution-polymerized types Evaluation proceduresCaoutchouc butadine-styrne (SBR)
5、Types polymriss en mulsion et en solution Mthode dvaluationINTERNATIONAL STANDARDISO2322Sixth edition2014-03-15Reference numberISO 2322:2014(E)BS ISO 2322:2014ISO 2322:2014(E)ii ISO 2014 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2014All rights reserved. Unless otherwise specified, no part
6、of this publication may 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
7、 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 www.iso.orgPublished in SwitzerlandBS ISO 2322:2014ISO 2322:2014(E) ISO 2014 All rights reserved iiiContents PageForeword iv1 Scope . 12 Normati
8、ve references 13 Sampling and further preparative procedures . 24 Physical and chemical tests on raw rubber 24.1 Mooney viscosity . 24.2 Volatile matter . 24.3 Ash . 25 Preparation of the test mixes 25.1 Standard test formulations . 25.2 Alternative formulations for oil-extended types . 35.3 Procedu
9、re 46 Evaluation of vulcanization characteristics by a curemeter test . 86.1 Using an oscillating-disc curemeter 86.2 Using a rotorless curemeter 87 Evaluation of tensile stress-strain properties of vulcanized test mixes . 88 Precision . 89 Test report . 9Annex A (informative) Precision 10Annex B (i
10、nformative) Examples .15Bibliography .16BS ISO 2322:2014ISO 2322:2014(E)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 techn
11、ical committees. Each member body interested in a subject for which a technical 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
12、with the International Electrotechnical Commission (IEC) on all matters 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 neede
13、d for the different types of ISO documents should be noted. This document 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 ri
14、ghts. ISO shall not be held responsible for identifying any or all such 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 th
15、is document is information given for the convenience of users and does not 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 t
16、o Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee 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 (
17、ISO 2322:2009), which has been technically revised. In particular: 5.3.1 states that the laboratory internal mixer procedure is the preferred method; Note 2 in 5.3.3 has been updated for more clarity.iv ISO 2014 All rights reservedBS ISO 2322:2014INTERNATIONAL STANDARD ISO 2322:2014(E)Styrene-butadi
18、ene rubber (SBR) Emulsion- and solution-polymerized types Evaluation proceduresWARNING 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
19、 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 specifies: physical and chemical tests on raw rubbers; standard materials, standard test formulations, equipment
20、, and processing methods for evaluating the vulcanization characteristics of emulsion- and solution-polymerized styrene-butadiene rubbers (SBR), including oil-extended rubbers.It applies to those rubbers listed in Table 1 which are normally used in vulcanized form.Table 1 Types of raw styrene-butadi
21、ene rubberRubber (oil-extended or non-oil-extended)StyreneType of copolymerTotal content % mass fractionBlock content % mass fractionSeries AEmulsion SBRSolution SBRSolution SBRRandomRandomPartial block5050500030Series BEmulsion SBRSolution SBRSolution SBRRandomRandomPartial block50505000302 Normati
22、ve 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, the latest edition of the referenced document (including any amendments) app
23、lies.ISO 37, Rubber, vulcanized or thermoplastic Determination of tensile stress-strain propertiesISO 247:2006, 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 co
24、ntent Part 2: Thermogravimetric methods using an automatic analyser with an infrared drying unit ISO 2014 All rights reserved 1BS ISO 2322:2014ISO 2322:2014(E)ISO 289-1, Rubber, unvulcanized Determinations using a shearing-disc viscometer Part 1: Determination of Mooney viscosityISO 1795, Rubber, ra
25、w 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 curem
26、etersISO 23529, Rubber General procedures for preparing and conditioning test pieces for physical test methods3 Sampling and further preparative procedures3.1 Take a laboratory sample of approximately 1,5 kg by the method described in ISO 1795.3.2 Prepare test samples in accordance with ISO 1795.4 P
27、hysical and chemical tests on raw rubber4.1 Mooney viscosityDetermine the Mooney viscosity in accordance with ISO 289-1 on a test sample prepared in accordance with the preferred method of ISO 1795 (unmilled test sample). Record the result as ML(1 + 4) at 100 C.If ML(1 + 4) at 100 C exceeds 100 Moon
28、ey units, the small rotor can be used and the result reported as MS(1 + 4) at 100 C.Alternatively, the Mooney viscosity can be determined on a test sample prepared by the mill massing procedure of ISO 1795. However, this method gives poorer reproducibility and the results might be different.4.2 Vola
29、tile matterDetermine the volatile-matter content by the hot-mill method or by the oven method as specified in ISO 248-1 and ISO 248-2.4.3 AshDetermine the ash in accordance with method A or method B of ISO 247:2006.5 Preparation of the test mixes5.1 Standard test formulationsThe standard test formul
30、ations are given in Table 2.The materials shall be national or international standard reference materials.If no standard reference material is available, the materials to be used shall be agreed by the parties concerned.2 ISO 2014 All rights reservedBS ISO 2322:2014ISO 2322:2014(E)Table 2 Test formu
31、lationsMaterialParts mass fractionSeries A Series BStyrene-butadiene rubber (SBR) (including oil in oil-extended SBR)100,00 Standard SBR 1500aSeries B SBRSulfurStearic acidIndustry reference blackbZinc oxideTBBSc1,751,0050,003,001,0065,0035,001,751,0035,003,001,00Total 156,75 141,75aThe previously u
32、sed SBR 1500 EST is no longer available. It is therefore necessary to use another commercially available SBR 1500. The type shall be agreed between the interested parties.bUse the current industrial reference black. Dry the material for 1 h at 125 C 3 C and store in a tightly closed container.cN-ter
33、t-butylbenzothiazole-2-sulfenamide. This is supplied in powder form having an initial insoluble-matter content, determined in accordance with ISO 11235, of less than 0,3 %. The material shall be stored at room temperature in a closed container and the insoluble matter checked every 6 mo. If this is
34、found to exceed 0,75 %, the material shall be discarded or recrystallized.5.2 Alternative formulations for oil-extended typesASTM D 3185 specifies the test formulations given in Table 3 for evaluation of general-purpose, oil-extended SBR, depending on the oil content of the rubber. These test formul
35、ations can be used as alternatives to the test formulations given in Table 2.Table 3 Alternative test formulations for oil-extended typesQuantity mass fractionFormulation number 1B 2B 3B 4B 5B 6BParts of oil 25 37,5 50 62,5 75 YaOil-extended rubberZinc oxideSulfurStearic acidIndustry reference black
36、bTBBSc125,003,001,751,0062,501,25137,503,001,751,0068,751,38150,003,001,751,0075,001,50162,503,001,751,0081,251,63175,003,001,751,0087,501,75100 + Y3,001,751,00(100 + Y)/2(100 + Y)/100Total 194,50 213,38 232,25 251,13 270,00aY = parts of oil, mass fraction, per 100 parts of base polymer in the oil-e
37、xtended rubber.bUse the current industrial reference black. Dry the material for 1 h at 125 C 3 C and store in a tightly closed container.cN-tert-butylbenzothiazole-2-sulfenamide. This is supplied in powder form having an initial insoluble-matter content, determined in accordance with ISO 11235, of
38、less than 0,3 %. The material shall be stored at room temperature in a closed container and the insoluble matter checked every 6 months. If this is found to exceed 0,75 %, the material shall be discarded or recrystallized. ISO 2014 All rights reserved 3BS ISO 2322:2014ISO 2322:2014(E)5.3 Procedure5.
39、3.1 Equipment and procedureThe equipment and procedure for the preparation, mixing, and vulcanization shall be in accordance with ISO 2393.Three alternative mixing procedures are specified, but in accordance with ISO 2393, the laboratory internal mixer procedure is preferred. Method A: mill mixing.
40、Method B: single-stage mixing using a laboratory internal mixer (the preferred procedure). Method C: two-stage mixing using a laboratory internal mixer for initial mixing and a mill for final mixing.5.3.2 Method A Mill-mixing procedureThe standard laboratory mill batch mass, in grams, shall be based
41、 on four times the formulation mass (i.e. 4 156,75 g = 627 g or 4 141,75 g = 567 g). Maintain the surface temperature of the rolls at 50 C 5 C. Maintain a good rolling bank at the nip of the rolls during mixing. If this is not obtained with the nip settings specified hereunder, small adjustments to
42、the mill openings might be necessary.Series A Series BDuration (min)Cumulative time (min)Duration (min)Cumulative time (min)a) Homogenize series B rubbers with the mill opening set at 1,1 mm at a temperature of 100 C 5 C. 1,0 1,0b) Band the rubber with the mill opening set at 1,1 mm and make 3/4 cut
43、s every 30 s from alternate sides.7,0 7,0 After banding the SBR 1500, add the rubber homogenized as in step a) above and make 3/4 cuts from both sides every 30 s. 8,0 9,0c) Add the sulfur slowly and evenly across the rubber.2,0 9,0 2,0 11,0d) Add the stearic acid. Make one 3/4 cut from each side.2,0
44、 11,0 2,0 13,0e) Add the carbon black evenly across the mill at a uniform rate. When about half the black has been incorporated, open the mill to 1,4 mm and make one 3/4 cut from each side. Then add the remainder of the carbon black. Be certain to add any black that has dropped into the mill pan. Wh
45、en all the black has been incorporated, open the mill to 1,8 mm and make one 3/4 cut from each side.12,0 23,0 12,0 25,04 ISO 2014 All rights reservedBS ISO 2322:2014ISO 2322:2014(E)f) Add the zinc oxide and the TBBS with the mill opening still at 1,8 mm.3,0 26,0 3,0 28,0g) Make three 3/4 cuts from e
46、ach side. 2,0 28,0 2,0 30,0h) Cut the batch from the mill. Set the mill opening to 0,8 mm and pass the rolled batch endwise through the rolls six times.2,0 30,0 2,0 32,0i) Sheet the batch to an approximate thickness of 6 mm by opening the mill and passing the stock through the mill four times, foldi
47、ng it back on itself each time. Determine the mass of the batch in accordance with ISO 2393. If the mass of the batch differs from the theoretical value by more than +0,5 % or 1,5 %, discard the batch and remix. Remove sufficient material for curemeter testing.j) Sheet the batch to approximately 2,2
48、 mm for preparing test sheets or to the appropriate thickness for preparing ISO ring test pieces in accordance with ISO 37.k) Condition the batch for 2 h to 24 h after mixing and prior to vulcanizing, if possible at standard temperature and humidity as defined in ISO 23529.5.3.3 Method B Single-stag
49、e mixing using a laboratory internal mixerFor 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 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-conditi
