1、BSI Standards PublicationBS ISO 13317-4:2014Determination of particle sizedistribution by gravitationalliquid sedimentation methodsPart 4: Balance methodBS ISO 13317-4:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 13317-4:2014.The UK participation in its
2、 preparation was entrusted to TechnicalCommittee LBI/37, Particle characterization including sieving.A list 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 resp
3、onsible for its correctapplication. The British Standards Institution 2014. Published by BSI StandardsLimited 2014ISBN 978 0 580 77138 5ICS 19.120Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Po
4、licy and Strategy Committee on 30 November 2014.Amendments issued since publicationDate Text affectedBS ISO 13317-4:2014 ISO 2014Determination of particle size distribution by gravitational liquid sedimentation methods Part 4: Balance methodDtermination de la distribution granulomtrique par les mtho
5、des de sdimentation par gravit dans un liquide Partie 4: Mthode de la balanceINTERNATIONAL STANDARDISO13317-4First edition2014-11-15Reference numberISO 13317-4:2014(E)BS ISO 13317-4:2014ISO 13317-4:2014(E)ii ISO 2014 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2014All rights reserved. Unless
6、 otherwise specified, no part 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 add
7、ress below or ISOs member body 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 13317-4:2014ISO 13317-4:2014(E) ISO 2014 All rights reserved iiiContents
8、 PageForeword ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Symbols 25 Principle of Method . 26 Measurement apparatus 37 Measuring method 47.1 Measurement of density . 47.2 Preparation method of suspension . 47.3 Measurement 57.4 Data analysis . 68 Accuracy 89 Size
9、range of measurement . 810 Data representation 8Annex A (informative) Data reduction by matrix method 10Bibliography .14BS ISO 13317-4:2014ISO 13317-4:2014(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). T
10、he 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 that committee. International organizations, governmental and non-go
11、vernmental, 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 document and those intended for its further maintenance are described
12、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 Directives, Part 2 (see www.iso.org/directives).Attention is drawn to the
13、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 development of the document will be in the Introduction and/or on the ISO li
14、st 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 specific terms and expressions related to conformity assessment, as well
15、 as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT), see the following URL: Foreword Supplementary information.The committee responsible for this document is ISO/TC 24, Particle characterization including sieving, Subcommittee SC 4, Particle characteri
16、zation.ISO 13317 consists of the following parts, under the general title Determination of particle size distribution by gravitational liquid sedimentation methods: Part 1: General principles and guidelines Part 2: Fixed pipette method Part 3: X-ray gravitational technique Part 4: Balance methodiv I
17、SO 2014 All rights reservedBS ISO 13317-4:2014ISO 13317-4:2014(E)IntroductionThis document is a part of the ISO 13317 series. It describes a method to determine particle size distribution by use of the mass of particles deposited at a balance. This method is based on a direct mass measurement and gi
18、ves immediately the mass-based distribution of particle diameter. This method does not use any fitting parameters. The results obtained are Stokes diameters. ISO 2014 All rights reserved vBS ISO 13317-4:2014BS ISO 13317-4:2014Determination of particle size distribution by gravitational liquid sedime
19、ntation methods Part 4: Balance method1 ScopeThis part of ISO 13317 specifies the method for the determination of particle size distribution by the mass of particles settling under gravity in liquid. This method is based on a direct mass measurement and gives the mass distribution of equivalent sphe
20、rical particle diameter. Typically, the gravitational liquid sedimentation method applies to samples in the 1 m to 100 m size range and where the sedimentation condition for particle Reynolds number less than 0,25 is satisfied.2 Normative referencesThe following documents, in whole or in part, are n
21、ormatively 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 9276-1, Representation of results of particle size anal
22、ysis Part 1: Graphical representationISO 13317-1, Determination of particle size distribution by gravitational liquid sedimentation methods Part 1: General principles and guidelinesISO 14887, Sample preparation Dispersing procedures for powders in liquidsISO 14488, Particulate materials Sampling and
23、 sample splitting for the determination of particulate properties3 Terms and definitionsFor the purposes of this document, the terms and definitions given in ISO 13317-1 and the following apply.3.1apparent particle densityparticle mass divided by the volume it would occupy including all internal por
24、esINTERNATIONAL STANDARD ISO 13317-4:2014(E) ISO 2014 All rights reserved 1BS ISO 13317-4:2014ISO 13317-4:2014(E)4 SymbolsFor the purposes of this part of ISO 13317, the following symbols apply.Quantity Symbol Unit Derivative UnitMass of dispersion medium mlkg Maximum amount of sample same as the fi
25、rst line mskg Apparent particle density skg m-3Liquid density lkg m-3Cumulative mass for particle diameter greater than xiMikgTotal mass of particles MmaxkgSedimentation time for particle having a diameter xiand time, respectivelyti, t s Particle diameter xim Liquid viscosity Pa sSedimentation dista
26、nce h mGravity acceleration g m s-2Cumulative distribution by mass for particle diameter xiQ3,idimensionless Sedimentation mass at time tiand tend, respectively Gti, Gendkg Particle diameter corresponding to time t required to move distance hx m Maximum particle diameter xmaxm Sedimentation velocity
27、 v (x) m s-1Response function g (t,x) dimensionless Distribution density by mass q3(x) m-1Distribution density by mass at time tiq3,i(x) m-1Parameter defined by Formula (A.6) i(k)dimensionless 5 Principle of MethodThis method is based on particle settling in a gravitational field and uniformly dispe
28、rsed particles at start (homogeneous technique). The relationship between settling velocity v, that means the time t required to settle the distance h, is defined by the following formula according to Stokes law.vhtgx=()sl218(1)From Formula (1), the Stokes diameter x is directly obtained.xhgt=()18sl
29、(2)The above formulae can be applied for Reynolds numbers of sedimenting particles less than 0,25. The determination of the particle size by gravitational sedimentation is a cumulative method (see ISO 13317-1). In this case, the method determines the rate at which solid particles settle from the sus
30、pension in a known volume of cylindrical vessel to a given distance. The mass of particles settled at time t is summed up from the mass of all particles of a diameter greater than x and in part of particles of diameters less than x. This method does not use any fitting parameters to obtain particle
31、size distribution.2 ISO 2014 All rights reservedBS ISO 13317-4:2014ISO 13317-4:2014(E)6 Measurement apparatusa) Measurement apparatus to obtain the mass of the sedimentThe apparatus measures continuously the increase of the mass of the particles sedimented out from the suspension. The apparatus show
32、n in Figure 1 a) typically consists of a sedimentation container and mass measuring system (see Reference 2). Figure 1 b) shows other type of sedimentation tray (see Reference 3). For the mass measurement apparatus (electronic balance), detection precision shall be at least 1 % of the total mass of
33、particles in the detection tray.a) b)Key1 controller 7 main inlet pipe2 stirrer 8 bypass3 dispersion bath 9 sedimentation container4 valve 10 detection tray5 precision electronic balance 11 personal computer6 glove boxFigure 1 Measurement apparatus Sedimentation balance for particles in liquidb) Sed
34、imentation bathA typical sedimentation bath is shown in Figure 2. The detection tray has a cylindrical side wall and the clearance between the side wall of the tray and sedimentation bath shall be large enough to avoid interaction between them. Dimensions for the tray are shown in Figure 2. The foll
35、owing ratios should apply: 0881152,/,hd 11514822,/,;hd 04307112,/,dd 06109012,/,.hd ISO 2014 All rights reserved 3BS ISO 13317-4:2014ISO 13317-4:2014(E)Key1 support wire2 suspension3 sedimentation bath4 detection trayh sedimentation distanceFigure 2 Detection containerc) Dispersion bathIn the bath,
36、the particles have to be dispersed before measurement and the dispersion state has to be checked (see ISO 14887).d) Measuring systemFigure 1 shows a schematic diagram of the measuring system. By use of a time-controlled valve (key 4), a precision electronic balance (key 5), and a personal computer (
37、key 11), the cumulative mass of the sediment on the tray is automatically recorded.7 Measuring method7.1 Measurement of densityThe apparent particle density for the setting shall be measured (refer to ISO 13317-1:2001, 5.4).7.2 Preparation method of suspensionA representative sample according to ISO
38、 14488 shall be dispersed according to ISO 14887 in a dispersion medium.7.2.1 Dispersion mediumWhen the test particles are not well dispersed by the dispersion medium, it is necessary to use a suitable dispersing agent. In this case, the dispersion medium should satisfy the following requirements.a)
39、 Viscosity of the dispersion medium has to be in a suitable range regarding the sedimentation time.4 ISO 2014 All rights reservedBS ISO 13317-4:2014ISO 13317-4:2014(E)b) Flocculation and agglomeration shall be avoided also during sedimentation process.c) In the dispersion medium, the solid phase sha
40、ll be insoluble, chemically and hydro-dynamically stable, and not change its volume.d) Avoid using volatile liquid as sedimentation medium.7.2.2 SuspensionA suitable amount of test particles, dispersion medium, and if necessary, a dispersion agent shall be well mixed in the dispersion bath.The volum
41、e concentration of test particles in the dispersion medium should be less than 0,1 %. At higher volume concentrations, the hindrance function accounting for the hydrodynamic hindered settling effect has to be taken into account. Particle settling velocity reads:vhtgxf=()()sl218(3)where f() is the sa
42、mple specific hindrance function (see ISO 13317-1) and is liquid volume fraction defined by=()+()=111wwwsls(4)The values of and w are particle volume fraction and mass fraction, respectively.7.3 MeasurementThe following procedures shall be performed to take a measurement.a) Have the dispersion mediu
43、m prepared. The temperature of the dispersion medium should be constant during the preparation and measurement (see Annex A). Initial particle mass of W gram is given into a small beaker and 10 cm3of dispersion medium is directly added to the test particles and well mixed to prepare a pre-suspension
44、. After adding the appropriate amount of dispersing medium, the supersonic vibration is applied to the pre-suspension. Finally the necessary amount of dispersion medium has to be added, and the suspension has to be well mixed. After stirring of the suspension, it is supplied to the sedimentation bat
45、h and the measurement is started. During the preparation and the supply of the suspension to the dispersion bath, air bubbles shall be avoided.b) The measurement is stopped when all particles are settled down and the mass of sediment shows no further increase. In the case that fines are still suspen
46、ded in the dispersion, the suspension is sampled with a siphon. After drying the suspension, the mass of the fines is determined. ISO 2014 All rights reserved 5BS ISO 13317-4:2014ISO 13317-4:2014(E)Keyt time sx particle diameter mFigure 3 Typical sedimentation curve7.4 Data analysisFigure 3 depicts
47、a typical record from the balance indicating the mass increase of the sediment with time. This is the sedimentation curve G(t). In Figure 3, Giis the mass at the sedimentation time ti, and Miis the intercept of the tangential line at the point (ti, Gi) of the sedimentation curve. When the mass of se
48、diment reaches a constant value Gm(see Figure 3), maximum time, corresponding to the minimum Stokes diameter, is obtained assuming that all particles have the same apparent density.7.4.1 Differential methoda) Sedimentation times t1, t2 tncorresponding to particle diameters x1, x2 xnare calculated us
49、ing Formula (1).thgxisli=()182(5)wheretiis the sedimentation time (s);h is the sedimentation distance from water surface to the bottom of the detection tray (m); is the viscosity of dispersion medium (Pas);g is the gravity acceleration (m/s2);s, lare the densities of particle and dispersion medium, respectively (kg/m3);xiis the particle diameter corresponding to ti(Stokes diameter) (m).6 ISO 2014 All rights reservedBS ISO 13317-4:2014ISO 13317-
