1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationDD ISO/TS 16176:2011Rubber compoundingingredients Carbon black Determination of theaggregate-size distribution atultimate dispersionDD ISO/TS 16176:2011 DRAFT FOR DEVELOPMENTNati
2、onal forewordThis Draft for Development is the UK implementation of ISO/TS16176:2011.This publication is not to be regarded as a British Standard.It is being issued in the Draft for Development series of publicationsand is of a provisional nature. It should be applied on thisprovisional basis, so th
3、at information and experience of its practicalapplication can be obtained.Comments arising from the use of this Draft for Developmentare requested so that UK experience can be reported to theinternational organization responsible for its conversion toan international standard. A review of this publi
4、cation willbe initiated not later than 3 years after its publication by theinternational organization so that a decision can be taken on itsstatus. Notification of the start of the review period will be made inan announcement in the appropriate issue of Update Standards.According to the replies rece
5、ived by the end of the review period,the responsible BSI Committee will decide whether to support theconversion into an international Standard, to extend the life of theTechnical Specification or to withdraw it. Comments should be sentto the Secretary of the responsible BSI Technical Committee at Br
6、itishStandards House, 389 Chiswick High Road, London W4 4AL.The 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
7、secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2011ISBN 978 0 580 71141 1ICS 83.040.20Compliance with a British Standard cannot confer immunity fromlegal obligations.This Draft for Development wa
8、s published under the authority ofthe Standards Policy and Strategy Committee on 30 November 2011.Amendments issued since publicationDate Text affectedDD ISO/TS 16176:2011Reference numberISO/TS 16176:2011(E)ISO 2011TECHNICAL SPECIFICATION ISO/TS16176First edition2011-11-15Rubber compounding ingredie
9、nts Carbon black Determination of the aggregate-size distribution at ultimate dispersion Ingrdients de mlange du caoutchouc Noir de carbone Dtermination de la distribution de la taille des agrgats la dispersion ultime DD ISO/TS 16176:2011ISO/TS 16176:2011(E) COPYRIGHT PROTECTED DOCUMENT ISO 2011 All
10、 rights reserved. Unless otherwise specified, no part of this publication may be reproduced 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 o
11、f the 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 Switzerland ii ISO 2011 All rights reservedDD ISO/TS 16176:2011ISO/TS 16176:2011(E) ISO 2011 All rights reserved iiiContents Page
12、Foreword iv 1 Scope 1 2 Normative references 1 3 Significance and use . 1 4 Terms and definitions . 1 5 Apparatus . 3 6 Reagents 4 7 Sampling 4 8 Preparation of carbon black dispersion 5 9 Computer and software set-up 5 10 Procedure . 5 11 Precision 6 12 Test report 6 Annex A (informative) Precision
13、 statement 7 Bibliography 9 DD ISO/TS 16176:2011ISO/TS 16176:2011(E) iv ISO 2011 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally
14、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 that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the wo
15、rk. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare Inte
16、rnational Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. In other circumstances, particularly when there is a
17、n urgent market requirement for such documents, a technical committee may decide to publish other types of document: an ISO Publicly Available Specification (ISO/PAS) represents an agreement between technical experts in an ISO working group and is accepted for publication if it is approved by more t
18、han 50 % of the members of the parent committee casting a vote; an ISO Technical Specification (ISO/TS) represents an agreement between the members of a technical committee and is accepted for publication if it is approved by 2/3 of the members of the committee casting a vote. An ISO/PAS or ISO/TS i
19、s reviewed after three years in order to decide whether it will be confirmed for a further three years, revised to become an International Standard, or withdrawn. If the ISO/PAS or ISO/TS is confirmed, it is reviewed again after a further three years, at which time it must either be transformed into
20、 an International Standard or be withdrawn. 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/TS 16176 was prepared by Technical Committee ISO/TC 4
21、5, Rubber and rubber products, Subcommittee SC 3, Raw materials (including latex) for use in the rubber industry. This Technical Specification specifies a new test method to determine the aggregate-size distribution at ultimate dispersion. An interlaboratory test programme (ITP) was carried out but,
22、 because not enough of the laboratories had the necessary equipment, the results could not be used to validate the method. It is for this reason that ISO/TC 45/SC 3 decided to publish the document as a Technical Specification. When enough laboratories have the equipment, an ITP will be organized and
23、, assuming the result is satisfactory, the Technical Specification will be converted into an International Standard. DD ISO/TS 16176:2011TECHNICAL SPECIFICATION ISO/TS 16176:2011(E) ISO 2011 All rights reserved 1Rubber compounding ingredients Carbon black Determination of the aggregate-size distribu
24、tion at ultimate dispersion 1 Scope This Technical Specification specifies a method for determining the size distribution of carbon black aggregates dispersed in a liquid by means of a high-power ultrasonic device. The measurement is done with a disc centrifuge photosedimentometer. This technique is
25、 based on the hydrodynamic behaviour of carbon black in a centrifugal field. The determination of the aggregate-size distribution is important in the evaluation of carbon black used in the rubber industry. 2 Normative references The following referenced documents are indispensable for the applicatio
26、n 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 1124, Rubber compounding ingredients Carbon black shipment sampling procedures ISO 3696, Water for analytical labora
27、tory use Specification and test methods 3 Significance and use Disc centrifuge photosedimentometry produces a rapid mass-differential aggregate-size distribution by continuously measuring the solution turbidity as a function of centrifugation time. In order to obtain a true mass distribution, a ligh
28、t-scattering correction has to be applied. 4 Terms and definitions For the purposes of this document, the following terms and definitions apply. 4.1 carbon black aggregate discrete, rigid colloidal entity that is the smallest dispersible unit in a suspension NOTE It is composed of extensively coales
29、ced particles. 4.2 spin fluid inert liquid injected into the disc of a disc centrifuge photosedimentometer prior to the sample and through which aggregates sediment NOTE Alkaline conditions minimize agglomeration of dispersed aggregates in most cases. DD ISO/TS 16176:2011ISO/TS 16176:2011(E) 2 ISO 2
30、011 All rights reserved4.3 dispersion fluid liquid in which aggregates are dispersed 4.4 Stokes equation mathematical description of the sedimentation of a spherical particle: 16st2121,8 10 lnRSDtwhere Dstis the Stokes diameter (nm); is the viscosity of the spin fluid (Pas); R is the distance of the
31、 photodetector from the centre of rotation (cm); S is the distance of the air-liquid interface from the centre of rotation (cm); t is the time of centrifugation (s); 1is the density of the carbon black (mg/m3); 2is the density of the spin fluid (mg/m3); is the rotational velocity (rad/s). NOTE 1,86
32、109mg/m3is often used as a typical value for the carbon black density, 1. 4.5 Stokes diameter Dstdiameter of a sphere which sediments in a viscous medium in a centrifugal or gravitational field in accordance with the Stokes equation NOTE 1 A non-spherical object, such as a carbon black aggregate, ca
33、n also be represented in terms of an equivalent Stokes diameter if it is considered as behaving as a smooth, rigid sphere of the same density and with the same sedimentation rate as the object. NOTE 2 For carbon black, the Stokes diameter is expressed in nanometres (nm). 4.6 mode Stokes diameter dmo
34、devalue at which the most frequent diameter occurrence is observed, which is portrayed as a peak in the distribution curve NOTE In some cases, more than one peak can be observed. 4.7 average Stokes diameter dwx-value of the point on the mass distribution curve that corresponds to the average in mass
35、 of the distribution DD ISO/TS 16176:2011ISO/TS 16176:2011(E) ISO 2011 All rights reserved 35 Apparatus 5.1 Disc centrifuge photosedimentometer (DCP)1 ), capable of rotational speeds of 1 000 rpm to 10 000 rpm or greater, with integral spin feed-back control (accuracy and stability of rotational spe
36、ed better than 0,05 %), spin fluid volume from 10 cm3to 20 cm3, stable temperature of spin fluid, stroboscope to monitor the rotating disc both for stability and streaming anomalies, and an appropriate optical turbidity measuring device. 5.2 Probe-type sonicator2), rating 750 W. 5.2.1 This has been
37、found to be an effective means of dispersing material into discrete aggregates. A probe with a tip diameter of 13 mm is recommended. 5.2.2 To determine the optimum sonication time, sonicate industry tint reference black (ITRB)3). Sufficient deagglomeration of the reference black will give a peak at
38、72 nm 5 nm in the aggregate-size distribution. Vary the sonication time and the amplitude scale setting of the probe until this value is obtained. Use the same conditions when analysing carbon black samples. Repeat this procedure each time the probe tip is changed. NOTE With a 750 W probe-type sonic
39、ator, ultrasonic disintegration for 10 min at 60 % on the amplitude scale is normally sufficient. 5.2.3 Sonicator tips are consumed with time, therefore it is recommended a) to test a reference material (for example ITRB) before testing actual samples; b) to change the tip if the mode Stokes diamete
40、r is more than 5 nm higher than previously obtained values. 5.3 Analytical balance, capable of weighing to the nearest 0,1 mg. 5.4 Beaker, 50 cm3, tall-form. 5.5 Two 1 000 cm3volumetric flasks, one fitted with a 100 cm3dispenser. 5.6 Syringes, 1 cm3, 2 cm3and 20 cm3. 5.7 pH-meter. 5.8 Ice bath. 1) A
41、n example of a DCP instrument which has been found to be acceptable is the BI-DCP Particle Sizer, available from Brookhaven Instruments Corporation, 750 Blue Point Rd., Holtsville, NY 11742, USA. This information is given for the convenience of users of this Technical Specification and does not cons
42、titute an endorsement by ISO of the instrument named. Other instruments may be used provided they comply with the requirements specified. 2) A suitable example is the Model Vibra Cell 75043 Probe Sonicator, available from Sonics. This information is given for the convenience of users of this Technic
43、al Specification and does not constitute an endorsement by ISO of the apparatus named. Other apparatus may be used provided it complies with the requirements specified. 3) ITRB is available from Balentine Enterprises, Inc., 227 Somerset St., Borger, TX 79007, USA. This information is given for the c
44、onvenience of users of this Technical Specification and does not constitute an endorsement by ISO of the product named. Equivalent products may be used if they can be shown to give the same results. DD ISO/TS 16176:2011ISO/TS 16176:2011(E) 4 ISO 2011 All rights reserved6 Reagents Unless otherwise st
45、ated, use only reagents of recognized reagent grade4). 6.1 Water, distilled or deionized, grade 3 as defined in ISO 3696. 6.2 Ethanol, absolute. 6.3 Surfactant, non-ionic type5), 0,02 % to 0,05 % (by mass) solution. 6.4 Dodecane, purity 98 % (by mass) (GC grade). 6.5 0,1 M sodium hydroxide solution.
46、 6.6 Spin fluid, prepared as follows. Place approximately 0,5 g of surfactant, weighed to the nearest 0,1 mg, in a 1 l volumetric flask. Make up to the mark with distilled or deionized water and homogenize. Use a pH-meter to check that the pH is between 9 and 10. If this is not the case, adjust the
47、pH with 0,1 M sodium hydroxide solution. 6.7 Dispersion fluid, prepared as follows. Place approximately 0,5 g of surfactant, weighed to the nearest 0,1 mg, in a 1 l volumetric flask. Make up to the mark with a distilled or deionized water/ethanol mixture (80/20 by volume) and homogenize. Use a pH-me
48、ter to check that the pH is between 9 and 10. If this is not the case, adjust the pH with 0,1 M sodium hydroxide solution. 7 Sampling Select carbon black samples from larger-sized lots at random, in either pelletized or non-pelletized form, in accordance with ISO 1124. Label the samples for analysis
49、 or for storage and subsequent analysis. 4) See Reagent Chemicals: American Chemical Society Specifications, American Chemical Society, Washington DC, USA. For suggestions on the testing of reagents not listed by the American Chemical Society, see Reagent Chemicals and Standards, by Joseph Rosin, D. Van Nostrand Co., Inc., New York, USA, and the United States Pharmacopeia. 5) Nonidet P-40, from Shell Chemicals, has been found suitable for this test method. This information is given for the convenience
