1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS ISO 4656:2012Rubber compoundingingredients Carbon black Determination of oilabsorption number (OAN)and oil absorption number ofcompressed sample (COAN)BS ISO 4656:2012 BRITISH
2、 STANDARDNational forewordThis British Standard is the UK implementation of ISO 4656:2012. Itsupersedes BS ISO 4656:2007 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee PRI/50, Rubber - Raw, natural and synthetic, includinglatex and carbon black.A list
3、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. Users are responsible for its correctapplication. The British Standards Institution 2012. Published by BSI StandardsLimite
4、d 2012ISBN 978 0 580 77727 1ICS 83.040.20Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 31 August 2012.Amendments issued since publicationDate Text affectedBS ISO
5、 4656:2012 ISO 2012Rubber compounding ingredients Carbon black Determination of oil absorption number (OAN) and oil absorption number of compressed sample (COAN)Ingrdients de mlange du caoutchouc Noir de carbone Dtermination de lindice dabsorption dhuile (OAN) et de lindice dabsorption dhuile dchant
6、illons comprims (COAN)INTERNATIONAL STANDARDISO4656Second edition2012-07-15Reference numberISO 4656:2012(E)BS ISO 4656:2012ISO 4656:2012(E)ii ISO 2012 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2012All rights reserved. Unless otherwise specified, no part of this publication may be reproduce
7、d or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing 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 1
8、1Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 4656:2012ISO 4656:2012(E) ISO 2012 All rights reserved iiiContents PageForeword iv1 Scope 12 Normative references . 13 Principle . 14 Reagents 25 Apparatus 26 Sample preparation . 37 Conditions of test 38 Proc
9、edure 38.1 Checking of the absorptometer and constant-rate burette . 38.2 Calibration and normalization of the absorptometer . 38.3 Test portion . 48.4 Determination . 59 Expression of results . 510 Precision and bias . 511 Test report . 5Annex A (normative) Preparation of compressed test portions 7
10、Annex B (normative) Checking and adjustment of torque and hydraulic damping .12Annex C (normative) Checking of the constant-rate burette 14Annex D (informative) Precision and bias16Bibliography .18BS ISO 4656:2012ISO 4656:2012(E)ForewordISO (the International Organization for Standardization) is a w
11、orldwide 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
12、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 electrotechnical standardization.International Standards are drafted
13、 in accordance with the rules given in the ISO/IEC Directives, Part 2.The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standar
14、d requires approval by at least 75 % of the member bodies casting a vote.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.ISO 4656 was prepared by Tech
15、nical Committee ISO/TC 45, Rubber and rubber products, Subcommittee SC 3, Raw materials (including latex) for use in the rubber industry.This second edition cancels and replaces the first edition (ISO 4656:2007), which has been technically revised. In addition to a number of minor editorial changes,
16、 the following changes have been made: a warning concerning the dangers of dibutyl phthalate has been added at the beginning of Clause 4; the current standard reference black, SBR D8, has been added to Table 1; in A.3.7, “mesh” has been replaced by “nominal size of openings”; in Annex A concerning t
17、he preparation of compressed test portions, A.5.1.2, A.5.1.11, A.5.2.1 and A.5.2.14 have been rewritten to specify, for each type of carbon black, the mass of carbon black to be taken for the compression procedure and the mass to be subsequently taken as the test portion for determination of the abs
18、orption number of the compressed sample; the precision data (previously in Clause 10) have been moved to an informative annex (Annex D);ISO/TR 9272:2005 has been moved from the normative references clause to a bibliography.iv ISO 2012 All rights reservedBS ISO 4656:2012INTERNATIONAL STANDARD ISO 465
19、6:2012(E)Rubber compounding ingredients Carbon black Determination of oil absorption number (OAN) and oil absorption number of compressed sample (COAN)WARNING Persons using this International Standard should be familiar with normal laboratory practice. This standard does not purport to address all o
20、f 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 ScopeOil absorption number (OAN) is a measure of the ability of a carbon black to absor
21、b liquids. This property is a function of the structure of the carbon black. Either dibutyl phthalate (DBP) or paraffin oil is acceptable for use with standard pelleted grades, including N-series carbon blacks found in ASTM D1765, although OAN testing using paraffin oil on some speciality blacks and
22、 powder blacks might result in unacceptable differences as compared to OAN testing using DBP oil. While studies have shown the two oils to give comparable precision, paraffin oil offers the advantage of being non-hazardous.This International Standard specifies a method using an absorptometer for the
23、 determination of the oil absorption number of carbon black for use in the rubber industry.The same method is used for the determination of the oil absorption number of compressed samples of carbon black. The procedure for the preparation of the compressed samples is described in Annex A.2 Normative
24、 referencesThe following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 1126, Rubber compounding ingredient
25、s Carbon black Determination of loss on heatingASTM D1765, Standard Classification System for Carbon Blacks Used in Rubber ProductsASTM D4821, Standard Guide for Carbon Black Validation of Test Method Precision and Bias3 PrincipleOil is added to a test portion of the carbon black which is kept in mo
26、tion by means of rotating blades. As the liquid is added, the mixture changes from a free-flowing powder to a semi-plastic mass. The end-point for the determination is reached when the torque resulting from this change in viscous properties attains either a preset value or a defined percentage of th
27、e maximum torque, calculated from the recorded torque curve. ISO 2012 All rights reserved 1BS ISO 4656:2012ISO 4656:2012(E)4 ReagentsWARNING Dibutyl phthalate is classified as a “substance of very high concern” (SVHC) as it is considered toxic for reproduction. Its use or marketing is regulated in s
28、ome countries. Wear suitable protective clothing. Replace by paraffin oil if technically feasible.4.1 Dibutyl phthalate, 25= 1,042 Mg/m3to 1,047 Mg/m3;or4.2 Paraffin oil, having a kinematic viscosity of 10 mm2/s to 34 mm2/s (10 cSt to 34 cSt) at 40 C.4.3 Standard reference blacks (SRBs).1)5 Apparatu
29、s5.1 Absorptometer2), consisting of the elements given in 5.2 to 5.5.Two different basic kinds of absorptometer are in use:a) electronic models (types C, E and DABS), equipped with a load cell and a digital torque indicator;b) mechanical models (types A and B), which are older models based on spring
30、s and mechanical torque indicators.Even though the mechanical instruments are no longer commercially available, they may still be used.5.2 Mixing chamber, stainless steel.Other chamber materials, such as soft- or hard-anodized aluminium, are acceptable provided they give an acceptable reading for SR
31、B F after calibration (see 8.2.9). The surface finish of the mixing chamber is critical for the maintainance of proper calibration, and the mixing chamber shall not be modified to achieve calibration.It is recommended that new replacement chambers be pre-polished for 16 h to minimize the effects of
32、chamber surface changes on calibration during their initial use.5.3 Motor-driven rotors, which fit into the mixing chamber (5.2) and rotate at a frequency of 13 rad/s (125 rpm).5.4 Torque-sensing device, consisting of a load cell for measuring the torque curve.Absorptometers of types C and DABS have
33、 an integrated data acquisition system for recording the torque curve and calculating the end-point. A type E absorptometer can be equipped with an external data acquisition system3). Absorptometers of types A and B use a spring and a dashpot having a damper control valve operating 1) Standard refer
34、ence blacks are available from Laboratory Standards and Technologies, 227 Somerset Street, Borger, TX 79007, USA, Tel/Fax: +1 806 273 3006, E-mail: , Web site: . This information is given for the convenience of users of this International Standard and does not constitute an endorsement by ISO of the
35、 products produced by this company.2) Suitable apparatus is available from Brabender GmbH SRB F6: (133,6 3,3) cm3/100 g; SRB F7: (129,3 2,0) cm3/100 g. After calibration, this setting shall not be changed.8.2.10 Note that, for type C, E and DABS absorptometers: the torque-sensing system is preset at
36、 3 s damping; if a data acquisition system is used, the values of subsequent determinations are automatically corrected by the software.8.2.11 For type A and B absorptometers: check that the speed selector (if fitted) of the torque-recording instrument is in the correct position; it is mandatory to
37、apply the normalization as described in 8.2.2 to 8.2.9 for the calculation of the correct values of the oil absorption number.8.3 Test portion8.3.1 OAN determinationsWeigh out, to the nearest 20 mg, a mass of dried carbon black in accordance with Table 1.Table 1 Mass of test portion for determinatio
38、n of oil absorptionType of carbon blackMass of test portiongN630, N642, N700 series, except N765 25N800 and N900 series, SRB D7 and SRB D8 40All other types (including N765) 20With high-bulk-density blacks which do not sufficiently fill the mixing chamber, it might be necessary to use a larger test
39、portion of carbon black, so that enough torque is developed to activate the torque limit switch.8.3.2 COAN determinationsSee Annex A.4 ISO 2012 All rights reservedBS ISO 4656:2012ISO 4656:2012(E)8.4 Determination8.4.1 Transfer the test portion (see 8.3) to the mixing chamber of the absorptometer, ca
40、librated as specified in 8.2.8.4.2 Replace the mixing-chamber cover.8.4.3 Check the reagent flow by swinging the delivery tube over the waste container and switching on. The burette (5.5) shall deliver an air-free stream of the oil (4.1 or 4.2), and the delivery tube shall be free of air bubbles. Sw
41、itch off. Re-centre the delivery tube over the mixing chamber and switch to “automatic feed”.8.4.4 Set the burette counter to zero. If a data acquisition system is used, this is done automatically by the system.8.4.5 Press the start button.8.4.6 Record the burette counter reading after the instrumen
42、t has stopped.8.4.7 Dismantle the mixing chamber and clean the blades of the rotors (5.3) and the mixing chamber with the spatula (5.9).The cleaning process may be simplified by adding some dry black and operating the absorptometer before dismantling while re-filling the burette.8.4.8 Re-assemble th
43、e mixing chamber.9 Expression of resultsThe oil absorption number OAN (or COAN, if the sample has been compressed prior to the test) of the carbon black, expressed in cubic centimetres per 100 g, is given by the following equation:OAN (or COAN) 100=VmwhereV is the volume, in cubic centimetres, of oi
44、l used (see 8.4.6);m is the mass, in grams, of the test portion (see 8.3).Normalize the measured value using the equation in 8.2.4.10 Precision and biasSee Annex D.11 Test reportThe test report shall include the following particulars:a) a reference to this International Standard;b) all details neces
45、sary for the complete identification of the sample;c) the drying temperature used (125 C);d) whether the carbon black was compressed before testing (COAN) or not (OAN); ISO 2012 All rights reserved 5BS ISO 4656:2012ISO 4656:2012(E)e) the conditions of test;f) the mass of the test portion used;g) the
46、 method used for the determination of the end-point (fixed torque-limit switch setting or 70 % of maximum torque);h) the value of the torque-limit switch setting;i) the results obtained from the individual determinations, and their average;j) the date of the test.6 ISO 2012 All rights reservedBS ISO
47、 4656:2012ISO 4656:2012(E)Annex A (normative) Preparation of compressed test portionsA.1 ScopeThis annex specifies procedures for the preparation of samples for the determination of the oil absorption number of compressed samples of carbon black for use in the rubber industry.A.2 PrincipleA quantity
48、 of dry carbon black is compressed four times at a pressure of 165 MPa and then the oil absorption number is determined as described in this International Standard.A.3 ApparatusA.3.1 Balance, accurate to 10 mg.A.3.2 Oven, gravity-convection type, capable of temperature regulation to within 1 C at 12
49、5 C and temperature uniformity within 5 C.A.3.3 Compression cylinder and piston (type A or B).A.3.4 Hydraulic press, electrically operated, having sufficient power to force the piston into the cylinder during compression of the sample at a rate of 4,2 mm/s and to attain a final pressure of 165 MPa on the sample.A.3.5 Spatula.A.3.6 Steel beaker.A.3.7 Sieve, 850 m nominal size of openings.A.3.8 Brush, 38 mm stiff bristle.A.3.9 Desiccator.A.4 Sample preparationDr
