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1、BS ISO 14703:2008 ICS 81.060.30 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW BRITISH STANDARD Fine ceramics (advanced ceramics, advanced technical ceramics) Sample preparation for the determination of particle size distribution of ceramic powders Licensed CopyChinese Univer
2、sity of Hong Kong, 11/04/2009 09:17, Uncontrolled Copy, (c) BSI This British Standard was published under the authority of the Standards Policy and Strategy Committee on 28 February 2009 BSI 2009 ISBN 978 0 580 65412 1 Amendments/corrigenda issued since publication DateComments BS ISO 14703:2008 Nat
3、ional foreword This British Standard is the UK implementation of ISO 14703:2008. The UK participation in its preparation was entrusted to Technical Committee RPI/13, Advanced technical ceramics. A list of organizations represented on this committee can be obtained on request to its secretary. This p
4、ublication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obligations. Licensed CopyChinese University of Hong Kong, 11/04/2009 09:17, Uncontrolled Copy, (
5、c) BSI BS ISO 14703:2008 Reference number ISO 14703:2008(E) ISO 2008 INTERNATIONAL STANDARD ISO 14703 Second edition 2008-04-15 Fine ceramics (advanced ceramics, advanced technical ceramics) Sample preparation for the determination of particle size distribution of ceramic powders Cramiques technique
6、s Prparation de lchantillon pour la dtermination de la rpartition granulomtrique des poudres cramiques Licensed CopyChinese University of Hong Kong, 11/04/2009 09:17, Uncontrolled Copy, (c) BSI BS ISO 14703:2008 ISO 14703:2008(E) PDF disclaimer This PDF file may contain embedded typefaces. In accord
7、ance with Adobes licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In downloading this file, parties accept therein the responsibility of not infringing Adobes lic
8、ensing policy. The ISO Central Secretariat accepts no liability in this area. Adobe is a trademark of Adobe Systems Incorporated. Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation parameters were optimized for printi
9、ng. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below. COPYRIGHT PROTECTED DOCUMENT ISO 2008 All rights reserved. Unless otherwise
10、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 of the requester. ISO copyright offi
11、ce 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 2008 All rights reserved Licensed CopyChinese University of Hong Kong, 11/04/2009 09:17, Uncontrolled Copy, (c) BSI BS ISO 14703:2008 ISO 14703:20
12、08(E) ISO 2008 All rights reserved iii Contents Page Foreword iv 1 Scope . 1 2 Normative references. 1 3 Terms and definitions. 1 4 Sampling 2 5 Dispersing media 2 6 Deagglomeration of sample. 4 7 Suspension and dispersion of sample. 4 8 Treatment of suspension. 5 9 Record of preparation conditions.
13、 5 Licensed CopyChinese University of Hong Kong, 11/04/2009 09:17, Uncontrolled Copy, (c) BSI BS ISO 14703:2008 ISO 14703:2008(E) iv ISO 2008 All rights reserved Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodie
14、s). 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 on that committee. International organizations, governmental and n
15、on-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 in accordance with the rules given in the ISO/IEC Directives, Pa
16、rt 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 Standard requires approval by at least 75 % of the member bodies castin
17、g 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 14703 was prepared by Technical Committee ISO/TC 206, Fine ceramics. This second editio
18、n cancels and replaces the first edition (ISO 14703:2000), which has been technically revised. Licensed CopyChinese University of Hong Kong, 11/04/2009 09:17, Uncontrolled Copy, (c) BSI BS ISO 14703:2008 INTERNATIONAL STANDARD ISO 14703:2008(E) ISO 2008 All rights reserved 1 Fine ceramics (advanced
19、ceramics, advanced technical ceramics) Sample preparation for the determination of particle size distribution of ceramic powders 1 Scope This International Standard specifies a general wet-sample preparation technique common to the size analysis of powdered fine ceramic materials. The analyzed size
20、distribution of fine particles is strongly dependent on the sample preparation. 2 Normative references The 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 re
21、ferenced document (including any amendments) applies. ISO 3696:1987, Water for analytical laboratory use Specification and test methods ISO 8213:1986, Chemical products for industrial use Sampling techniques Solid chemical products in the form of particles varying from powders to coarse lumps 3 Term
22、s and definitions For the purposes of this document, the following terms and definitions apply. 3.1 fine particles particles of which sizes are less than a few micrometres 3.2 sample preparation process that includes deagglomeration, dispersion of a test sample and treatment of suspension in stages
23、up to taking the test portion 3.3 test sample representative part taken from a quantity of material 3.4 test portion quantity of material taken from the test sample entirely used in the test 3.5 dispersing medium liquid in which the sample is dispersed and suspended 3.6 Na-HMP sodium hexametaphospha
24、te Licensed CopyChinese University of Hong Kong, 11/04/2009 09:17, Uncontrolled Copy, (c) BSI BS ISO 14703:2008 ISO 14703:2008(E) 2 ISO 2008 All rights reserved 4 Sampling The sampling method, from a quantity of material to the test sample, shall comply with the requirements specified in ISO 8213, o
25、therwise the methods specified in a national standard, or as mutually agreed upon, shall be complied with. 5 Dispersing media 5.1 Types of dispersing media 5.1.1 Aqueous solution of Na-HMP A solution of Na-HMP with a mass concentration of 0,01 % to 0,1 % should be used for the samples that are insol
26、uble or can be regarded as insoluble. The dispersing medium shall be used no more than two days after preparation. The water should be equivalent to the water of type 1 defined in ISO 3696. 5.1.2 Ethanol Ethanol of analytical grade or better should be used for samples soluble in, or reactive with, w
27、ater. 5.1.3 Other dispersing media In case sufficient dispersing effects are not obtained with Na-HMP water solution or ethanol, other dispersing media, such as polymer dispersant solution, can be used but the following conditions shall be satisfied. a) The dispersing medium shall not contain solid
28、or liquid particles. b) The dispersing medium shall wet the sample material thoroughly. c) The dispersion medium shall not cause the particulate material to dissolve, swell, shrink or coagulate. d) The dispersing medium shall not foam during ultrasonic agitation. e) Analytical grade or better reagen
29、ts shall be used for the dispersing medium. f) For wet sedimentation methods, the dispersing medium and the sample material shall have different densities. g) For the laser diffraction method, the dispersing medium and the sample material shall have different refractive indices. 5.2 Evaluation of di
30、spersed conditions for the selection of dispersing medium The evaluation of dispersed conditions should be made by one or more of the following techniques, for selection of the dispersant medium or the dispersant concentration. a) Measurement of zeta-potential: the greatest absolute value of zeta-po
31、tential, preferably more than 60 mV, is required. b) Observation of sedimentation process: no clear boundary between the supernatant and the settling suspension shall be detected (see Figure 1). c) Observation of sediment: the sediment shall be as dense as possible (see Figure 2). d) Measurement of
32、particle size distribution: the finest particle size distribution curve shall be obtained from the best dispersed particles. The method of zeta-potential measurement should comply with the methods specified in a national standard or as mutually agreed upon. Licensed CopyChinese University of Hong Ko
33、ng, 11/04/2009 09:17, Uncontrolled Copy, (c) BSI BS ISO 14703:2008 ISO 14703:2008(E) ISO 2008 All rights reserved 3 a) Well dispersed condition b) Poorly dispersed condition Figure 1 Sedimentation process a) Well dispersed condition b) Poorly dispersed condition Figure 2 Sediments Licensed CopyChine
34、se University of Hong Kong, 11/04/2009 09:17, Uncontrolled Copy, (c) BSI BS ISO 14703:2008 ISO 14703:2008(E) 4 ISO 2008 All rights reserved 6 Deagglomeration of sample 6.1 In order to improve the reproducibility of the size analysis, the test sample should be deagglomerated by means of a mortar and
35、pestle, using the following procedure. 6.2 The weighed sample is placed in a dry mortar. 6.3 The sample is strongly disintegrated with a pestle using the whole inner wall of the mortar until most of the sample adheres to it. 6.4 The sample adhering to the mortar wall is scraped off with a spatula or
36、 equivalent and collected at the bottom of the mortar. 6.5 The procedures in 6.3 and 6.4 are repeated five times. NOTE 1 Where it is known that the sample consists of separated primary particles, deagglomeration is not needed. NOTE 2 Deagglomeration is not needed to determine the particle size of th
37、e sample “as received” or “as is”. 7 Suspension and dispersion of sample 7.1 Suspension of sample The sample shall be suspended in the dispersing medium at a given concentration. The concentration shall be dilute but higher than the proper concentration for the instrumental technique used. As the be
38、aker capacity and the amount of suspension could affect the dispersing conditions, they shall be recorded. 7.2 Ultrasonic agitation of sample 7.2.1 Ultrasonic devices Dispersion of the sample shall be made with one of the following devices. a) Ultrasonic bath: the dispersion shall be made with the a
39、mount of water in the ultrasonic bath controlled in order to obtain the strongest dispersing effect, and with the beaker set at the position undergoing the strongest ultrasonic intensity. b) Ultrasonic homogenizer: the suspension shall not be contaminated by foreign particles generated from its tip.
40、 Its output, tip size and tip position may influence the dispersing condition and therefore shall be recorded. NOTE Where foreign particles are magnetic materials, they can be eliminated by mixing with a magnet stirrer. If the ultrasonic agitation causes a noticeable increase in temperature of more
41、than a few degrees Celsius, the samples should be cooled using water chilled with ice. 7.2.2 Ultrasonic agitation time The sample suspension shall be agitated until the obtained particle size, for example median diameter, becomes constant or minimum with the agitation time. If the obtained particle
42、size continues to decrease with the agitation time, the agitation can be stopped at a certain time at which the size analysis shall be conducted and recorded. NOTE Ultrasonic agitation is not needed for size analysis of the sample “as received” or “as is”. Licensed CopyChinese University of Hong Kon
43、g, 11/04/2009 09:17, Uncontrolled Copy, (c) BSI BS ISO 14703:2008 ISO 14703:2008(E) ISO 2008 All rights reserved 5 8 Treatment of suspension 8.1 Concentration control After ultrasonic agitation, and just before the size measurement, the concentration shall be adjusted, using the same dispersing medi
44、a, to the concentration suitable for the instrument technique. 8.2 Change with passage of time The suspension shall be kept agitated in order to prevent the sedimentation of coarse particles and reagglomeration when it is left to stand. If reagglomeration is not prevented by the agitation, the type
45、and concentration of dispersant should be re-examined. 8.3 Taking the test portion When a test portion is taken from the suspension of the test sample, the suspension shall be agitated sufficiently to avoid segregation. 9 Record of preparation conditions The conditions of sample preparation shall be
46、 recorded in detail. See the example in Table 1. Table 1 Conditions of sample preparation Date Operator Sample name Density g/cm3 Sample state Powder Slurry Particle properties Refractive index Sample history Na-HMP distilled water solution (0,01 % to 0,1 % by mass) Distilled water Maker Products Ot
47、hers Others % by mass, % by volume, distilled Water solution Ethanol Others Dispersion medium Viscosity mPas Density g/cm3 Refractive index Concentration of suspension Mass concentration g/ml (Sample g/Dispersion medium ml) Deagglomeration with mortar Dispersion device Material of mortar Ultrasonic
48、bath Ultrasonic homogenizer Mortar diameter mm Model W Hz Sample quantity g Material of tip Number of deagglomeration times Tip diameter mm Beaker used Position of tip head mm below suspension level Capacity ml Dispersion method Suspension volume ml Ultrasonic agitation time min Time from suspension
49、 min preparation to measurement Suspension temperature C Dilution ratio of suspension times for measurement Licensed CopyChinese University of Hong Kong, 11/04/2009 09:17, Uncontrolled Copy, (c) BSI BS ISO 14703:2008 ISO 14703:2008(E) ICS 81.060.30 Price based on 5 pages ISO 2008 All rights reserved Licensed CopyChinese University of Hong Kong, 11/04/2009 09:17, Uncontrolled Copy, (c) BSI BS ISO 14703:2008 This page has been intentionally left blank Licensed CopyChinese University of Hong Kong, 11/04/2009 09:17