1、BS ISO 15825:2017Rubber compoundingingredients Carbonblack Determination ofaggregate size distributionby disc centrifugephotosedimentometryBSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06BS ISO 15825:2017 BRITISH STANDARDNational forewordThis British Standard is the
2、UK implementation of ISO 15825:2017. It supersedes BS ISO 15825:2015 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee PRI/50, Raw materials (including latex) for use in the rubber industry.A list of organizations represented on this committee can be obt
3、ained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2017.Published by BSI Standards Limited 2017ISBN 978 0 580 92835 2 ICS 83.040.20 Compliance
4、with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 March 2017.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dBS ISO 15825:2017 ISO 2017Rubber com
5、pounding ingredients Carbon black Determination of aggregate size distribution by disc centrifuge photosedimentometryIngrdients de mlange de caoutchouc Noir de carbone Dtermination de la distribution dimensionnelle des agrgats par photosdimentomtrie avec centrifugeuse disqueINTERNATIONAL STANDARDISO
6、15825Third edition2017-03Reference numberISO 15825:2017(E)BS ISO 15825:2017ISO 15825:2017(E)ii ISO 2017 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2017, Published in SwitzerlandAll rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwi
7、se 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 officeCh.
8、de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgBS ISO 15825:2017ISO 15825:2017(E)Foreword iv1 Scope . 12 Normative references 13 Terms and definitions . 13.1 General terms . 13.2 Terms concerning aggregate dimensions 24 S
9、ignificance and use 35 Apparatus . 46 Reagents and materials . 47 Sampling 58 Calibration 59 Preparation of test sample . 510 Computer and software setup. 511 Initiation of procedure . 612 Test report . 7Annex A (informative) Example of a mass distribution curve . 8Annex B (informative) Precision .
10、9Bibliography .11 ISO 2017 All rights reserved iiiContents PageBS ISO 15825:2017ISO 15825:2017(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 carr
11、ied 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 work.
12、ISO collaborates closely 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 differen
13、t 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 Directives, Part 2 (see www .iso .org/ directives).Attention is drawn to the possibility that some of the elements of this document may
14、 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 development of the document will be in the Introduction and/or on the ISO list of patent declarations received (see www .iso .org/ pat
15、ents).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 specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the World Trade
16、 Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: www .iso .org/ iso/ foreword .htmlThis document was prepared by Technical Committee ISO/TC 45, Rubber and rubber products, Subcommittee SC 3, Raw materials (including latex) for use in the rubber industry.
17、This third edition cancels and replaces the second edition (ISO 15825:2015), which has been technically revised: to correct Figure A.1; to update the precision data in Annex B following a new interlaboratory trial programme (ITP) conducted in 2015 and 2016.iv ISO 2017 All rights reservedBS ISO 15825
18、:2017INTERNATIONAL STANDARD ISO 15825:2017(E)Rubber compounding ingredients Carbon black Determination of aggregate size distribution by disc centrifuge photosedimentometry1 ScopeThis document specifies a method for determining the size distribution of carbon black aggregates, using a disc centrifug
19、e photosedimentometer. This technique is 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 referencesThe following documents are refer
20、red to in the text in such a way that some or all of their content constitutes requirements 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 in
21、gredients Carbon black shipment sampling proceduresISO 3696, Water for analytical laboratory use Specification and test methods3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.ISO and IEC maintain terminological databases for use in standardization
22、at the following addresses: IEC Electropedia: available at h t t p :/ www .electropedia .org/ ISO Online browsing platform: available at h t t p :/ www .iso .org/ obp3.1 General terms3.1.1carbon black aggregatediscrete, rigid colloidal entity that is the smallest dispersible unit in a suspensionNote
23、 1 to entry: It is composed of extensively coalesced particles.3.1.2spin fluidinert liquid injected into the disc prior to the sample, through which aggregates sedimentNote 1 to entry: Alkaline conditions minimize agglomeration of dispersed aggregates in most cases.3.1.3dispersion fluidliquid in whi
24、ch aggregates are dispersed ISO 2017 All rights reserved 1BS ISO 15825:2017ISO 15825:2017(E)3.1.4Stokes equationmathematical description of the sedimentation of a spherical particle:DRStst161221,810=()lnwhereDstis the Stokes diameter (nm); is the viscosity of the spin fluid (Pas);R is the distance o
25、f the 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).3.1.5parti
26、cle densitydensity of the aggregate in Mg/m3Note 1 to entry: For carbon black, 1,86 103kg/m3(1,86 g/cm3) is used as a typical value.3.2 Terms concerning aggregate dimensions3.2.1Stokes diameterDstdiameter of a sphere which sediments in a viscous medium in a centrifugal or gravitational field accordi
27、ng to the Stokes equationNote 1 to entry: A non-spherical object, such as a carbon black aggregate, may 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
28、2 to entry: For carbon black, Stokes diameter is expressed in nanometres (nm).3.2.2mean diameteraverage diameterDmeanaverage diameter calculated from the differential mass distribution curveNote 1 to entry: It represents the first moment of the differential distribution.Note 2 to entry: In the softw
29、are of the Brookhaven disc centrifuge the mass distribution is called “Volume (Mass)” and mean diameter is reported as “Mean”.Note 3 to entry: Dmeanis used for reporting purposes only.2 ISO 2017 All rights reservedBS ISO 15825:2017ISO 15825:2017(E)3.2.3medianD50x-value of the point on the mass distr
30、ibution curve at which 50 % by mass of the test sample is larger and 50 % by mass of the test sample is smallerNote 1 to entry: It represents the median value of the distribution.Note 2 to entry: In the software of the Brookhaven disc centrifuge the median Stokes diameter is reported as “d50”.Note 3
31、 to entry: D50is used for reporting purposes only.3.2.4modeDmodevalue at which the most frequent diameter occurrence is observed, which is portrayed as a peak in the distribution curveNote 1 to entry: In some cases, there may be more than one mode indicated.Note 2 to entry: Dmodeis used for reportin
32、g purposes only.3.2.5lower quartilex-value of the point on the mass distribution curve at which 75 % of the sample is larger, and 25 % smaller3.2.6upper quartilex-value of the point on the mass distribution curve at which 75 % of the sample is smaller, and 25 % larger3.2.7quartile ratioratio of uppe
33、r quartile to lower quartileNote 1 to entry: In the software of the Brookhaven disc centrifuge the quartile ratio is reported as “d75/d25”.3.2.8D-50width of the plot of the mass distribution measured at the half-maximum point of the mode, which is a measure of the breadth of the aggregate size distr
34、ibutionNote 1 to entry: In the software of the Brookhaven disc centrifuge D 50 is reported as “FWHM” (full width at half maximum).4 Significance and useDisc centrifuge photosedimentometry produces a rapid mass-differential aggregate size distribution, by continuously measuring the solution turbidity
35、 as a function of centrifugation time. In order to obtain a true mass distribution, a light scattering correction shall be applied.An example of a mass distribution curve is given in Annex A. ISO 2017 All rights reserved 3BS ISO 15825:2017ISO 15825:2017(E)5 Apparatus5.1 Disc centrifuge photosediment
36、ometer (DCP)1), capable of rotational speeds of 1 000 r/min to 11 000 r/min or greater, with integral spin feed-back control (accuracy and stability of rotational speed better than 0,05 %), spin fluid volume from 10 cm3to 20 cm3, stable temperature of spin fluid, stroboscope to monitor the rotating
37、disc both for stability and streaming anomalies, and an appropriate optical turbidity measuring device.5.2 Energy meter, capable of measuring the energy consumption (in kWh) of the probe-type sonicator.The energy meter is inserted between an electrical plug of the laboratory and the plug of the powe
38、r supply cord of the sonicator. The actual energy consumption is indicated on a digital display.5.3 Probe-type sonicator2), typically with a nominal power of 200 W or more.The sonicator should be capable of providing a measured power consumption of at least 60 W. This has been found to be an effecti
39、ve means of dispersing carbon black into discrete aggregates. See Clause 8 for further details.NOTE Cylindrical tips with 12,7 mm (1/2 inch) diameter have been found to be suitable.6 Reagents and materialsUnless otherwise stated, use only reagents of recognized reagent grade3).6.1 Water, distilled o
40、r deionized, grade 3 as defined in ISO 3696.6.2 Ethanol, absolute.6.3 Surfactant, non-ionic type4), 0,02 % to 0,05 % (by mass) solution.6.4 Dodecane, 98 % purity (GC grade).6.5 Spin fluid: Water (6.1) containing surfactant (6.3) which may be adjusted to pH 9,0 to pH 10,0 using 0,1 mol/dm3NaOH.6.6 Di
41、spersion fluid: A solution of 20 cm3of ethanol (6.2) and 80 cm3of water (6.1) containing a surfactant (6.3). The solution may be adjusted to a pH value between 9,0 and pH 10,0 using 0,1 mol/dm3NaOH.1) BI-DCP Particle Sizer is available from Brookhaven Instruments Corporation, 750 Blue Point Rd., Hol
42、tsville, NY 11742, USA, www .brookhaveninstruments .com. Joyce Loebl DCF 4 is no longer available. It is an example of a suitable product available commercially. This information is given for the convenience of users of this document and does not constitute an endorsement by ISO of these products. 2
43、) Sonoplus 2220, equipped with Sonotrode UW 2200 and horn DH 13 G, is available from BANDELIN electronic GmbH b) a reference to this document, i.e. ISO 15825;c) the test parameters (sample mass, sonication time and energy, rotational speed of disc);d) the type of instrument and software used;e) the
44、test results based on the mass distribution (aggregate dimensional properties as defined in 4.6);f) any deviations from the procedure specified;g) any unusual features (anomalies) observed during the test;h) the date of the test. ISO 2017 All rights reserved 7BS ISO 15825:2017ISO 15825:2017(E)Annex
45、A (informative) Example of a mass distribution curveKey1 mode2 meanX diameterY cumulative/differential distributionNOTE DD7525= quartile ratioFigure A.1 Example of a mass distribution curve8 ISO 2017 All rights reservedBS ISO 15825:2017ISO 15825:2017(E)Annex B (informative) PrecisionB.1 The precisio
46、n of this test method was determined in accordance with ISO/TR 9272. Refer to this document for terminology and other statistical details.B.2 The precision results give an estimate of the precision to be expected. The precision parameters shall not be used for acceptance/rejection testing of any gro
47、up of materials without documentation that they are applicable to those particular materials and the specific testing protocols that include this test method.B.3 A type 1 precision interlaboratory trial programme was conducted. Both the repeatability and the reproducibility determined represent shor
48、t-term testing conditions. Thirteen laboratories tested four different carbon blacks on two different days in duplicate. However, not all the laboratories tested all the samples, therefore p 13, q = 4 and n = 4. A test result is the value obtained from a single determination. Acceptable difference v
49、alues were not measured.B.4 The results of the precision calculations are given in Table B.1, Table B.2. and Table B.3. Outliers have been removed. The number of laboratories remaining after outlier deletion is reported in Tables B.1 to B.3.Table B.1 Mean diameter, DmeanMaterialNumber of laboratoriesMean nmWithin laboratory Between laboratoriessrr (r) sRR (R)SRB-B8 (N134) 11 69,6 1,41 3,94 5,66 2,29 6,40 9,20ITRB (N330) 11 103,4 1,65 4,61 4,46 3,33 9,32 9,01ITRB-2 (N330) 10 101,4 1,46 4,09 4
