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1、 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 techniques Prparation de lchantil
2、lon pour la dtermination de la rpartition granulomtrique des poudres cramiques Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/25/2008 00:36:06 MDTNo reproduction or networking permitted without license
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6、t the address given below. COPYRIGHT PROTECTED DOCUMENT ISO 2008 All 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
7、either ISO at the address below or ISOs member body in the country of 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 2008 All rights reserved Copyright Internat
8、ional Organization for Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/25/2008 00:36:06 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 14703:2008(E) ISO 2008 All rights reserved iii Contents Page Foreword iv 1 Sco
9、pe . 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. 5 Copyright International Organization for Standardization Provided b
10、y IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/25/2008 00:36:06 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 14703:2008(E) iv ISO 2008 All rights reserved Foreword ISO (the International Organization for Standardization) is a worldwide
11、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 on that c
12、ommittee. 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 in acco
13、rdance 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 Standard requi
14、res 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 14703 was prepared by Technica
15、l Committee ISO/TC 206, Fine ceramics. This second edition cancels and replaces the first edition (ISO 14703:2000), which has been technically revised. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/25/
16、2008 00:36:06 MDTNo reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARD ISO 14703:2008(E) ISO 2008 All rights reserved 1 Fine ceramics (advanced ceramics, advanced technical ceramics) Sample preparation for the determination of particle size distribution of cer
17、amic 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 distribution of fine particles is strongly dependent on the sample preparation. 2 Normative references The following
18、 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 3696:1987, Water for analytical laboratory use Specificati
19、on 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 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 fine particles p
20、articles 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 up to taking the test portion 3.3 test sample representative part taken from a quantity of material 3.4 test portion
21、 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 hexametaphosphate Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Boeing C
22、o/5910770001 Not for Resale, 07/25/2008 00:36:06 MDTNo reproduction or networking permitted without license from IHS -,-,- 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
23、ISO 8213, otherwise 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 tha
24、t are insoluble 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 react
25、ive with, water. 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 con
26、tain solid 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 be
27、tter reagents 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 Evalu
28、ation of dispersed 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
29、 of zeta-potential, 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) Meas
30、urement of 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. Copyright International Organiz
31、ation for Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/25/2008 00:36:06 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 14703:2008(E) ISO 2008 All rights reserved 3 a) Well dispersed condition b) Poorly disperse
32、d condition Figure 1 Sedimentation process a) Well dispersed condition b) Poorly dispersed condition Figure 2 Sediments Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/25/2008 00:36:06 MDTNo reproduction
33、 or networking permitted without license from IHS -,-,- 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 pestle, using the following procedu
34、re. 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 equivalent and collected at the bo
35、ttom 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 the sample “as received” or “as is”.
36、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 beaker capacity and the amount of sus
37、pension 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 amount of water in the ultrasonic ba
38、th 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. Its output, tip size and tip posit
39、ion 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 than a few degrees Celsius, the sam
40、ples 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 size continues to decrease with the
41、 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”. Copyright International Organization for Standardization Provided by IHS under
42、 license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/25/2008 00:36:06 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 14703:2008(E) ISO 2008 All rights reserved 5 8 Treatment of suspension 8.1 Concentration control After ultrasonic agitation, and just befo
43、re the size measurement, the concentration shall be adjusted, using the same dispersing media, 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 reagglomerati
44、on when it is left to stand. If reagglomeration is not prevented by the agitation, the type 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 s
45、egregation. 9 Record of preparation conditions The conditions of sample preparation shall be 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
46、 Na-HMP distilled water solution (0,01 % to 0,1 % by mass) Distilled water Maker Products Others 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/Disper
47、sion medium ml) Deagglomeration with mortar Dispersion device Material of mortar Ultrasonic 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
48、ml Dispersion method Suspension volume ml Ultrasonic agitation time min Time from suspension min preparation to measurement Suspension temperature C Dilution ratio of suspension times for measurement Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/25/2008 00:36:06 MDTNo reproduction or networking permitted without license from IHS -,-