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1、INTERNATIONAL STANDARD ISO 13317-3 First edition 2001-03-01 Reference number ISO 13317-3:2001(E) ISO 2001 Determination of particle size distribution by gravitational liquid sedimentation methods Part 3: X-ray gravitational technique Dtermination de la distribution granulomtrique par les mthodes de
2、sdimentation par gravit dans un liquide Partie 3: Mthode aux rayons X par gravit Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/21/2007 01:45:58 MDTNo reproduction or networking permitt
3、ed without license from IHS -,-,- ISO 13317-3:2001(E) ii ISO 2001 All rights reserved PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licens
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6、 it is found, please inform the Central Secretariat at the address given below. ISO 2001 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, elec- tronic or mechanical, including photocopying and microfilm, without p
7、ermission in writing from either ISO at the address below or ISOs mem- ber 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.ch Web www.iso.ch Printed in Switzerland Copyright International Or
8、ganization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/21/2007 01:45:58 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 13317-3:2001(E) ISO 2001 All rights reserved iii ContentsPage 1Scope
9、.1 2Normative references .1 3Terms and definitions 1 4Symbols 2 5Sampling .2 6Representation of results 2 7Principle 2 8Apparatus .3 9Sample preparation 5 10Procedure .5 11Tests in duplicate, validation and verification 6 12Calculation of results 7 13Test report 7 Annex AExample of typical report 9
10、Bibliography.11 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/21/2007 01:45:58 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 13317-3:2001(E) iv ISO 2001
11、 All rights reserved Foreword 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 carried out through ISO technical committees. Each member body interested in a
12、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. ISO collaborates closely with the International Electrotechnical Commission
13、 (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an Int
14、ernational Standard requires 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 part of ISO 13317 may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights.
15、International Standard ISO 13317-3 was prepared by Technical Committee ISO/TC 24,Sieves, sieving and other sizing methods, Subcommittee SC 4,Sizing by methods other than sieving. ISO 13317 consists of the following parts, under the general titleDetermination of particle size distribution by gravitat
16、ional liquid sedimentation methods: Part 1: General principles and guidelines Part 2: Fixed pipette method Part 3: X-ray gravitational technique Annex A of this part of ISO 13317 is for information only. Copyright International Organization for Standardization Provided by IHS under license with ISO
17、Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/21/2007 01:45:58 MDTNo reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARDISO 13317-3:2001(E) ISO 2001 All rights reserved 1 Determination of particle size distribution by gravitational liquid se
18、dimentation methods Part 3: X-ray gravitational technique SAFETY PRECAUTIONS This part of ISO 13317 does not purport to address all of the safety considerations associated with its use. It is the responsibility of the user of this part of ISO 13317 to establish appropriate safety and health practice
19、s and determine the applicability of the regulatory limitations prior to its use. 1Scope This part of ISO 13317 describes a method for the determination of the particle size distribution of a powder dispersed in a liquid using gravity sedimentation. The measurement of the concentration of solids set
20、tling in a liquid suspension is achieved by monitoring the incremental signal absorption from a beam of X-rays. The method of determining the particle size distribution described in this part of ISO 13317 is applicable to powders which can be dispersed in liquids or powders which are present in slur
21、ry form. The typical particle size range for analysis is from aboutto about. The method is used for materials containing particles of the same chemical composition which produce adequate X-ray opacity. 2Normative references The following normative documents contain provisions which, through referenc
22、e in this text, constitute provisions of this part of ISO 13317. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply. However, parties to agreements based on this part of ISO 13317 are encouraged to investigate the possibility of applying the most
23、recent editions of the normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 787-10,General methods of test for pigments and extenders Pa
24、rt 10: Determination of density Pyknometer method. ISO 8213,Chemical products for industrial use Sampling techniques Solid chemical products in the form of particles varying from powders to coarse lumps. ISO 9276-1,Representation of results of particle size analysis Part 1: Graphical representation.
25、 ISO 13317-1,Determination of particle size distribution by gravitational liquid sedimentation methods Part 1: General principles and guidelines. ISO 14887,Sample preparation Dispersing procedures for powders in liquids. 3Terms and definitions For the purposes of this part of ISO 13317, the terms an
26、d definitions given in ISO 13317-1 apply. 0,5m100m Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/21/2007 01:45:58 MDTNo reproduction or networking permitted without license from IHS -,
27、-,- ISO 13317-3:2001(E) 2 ISO 2001 All rights reserved 4Symbols For the purpose of this part of ISO 13317, the symbols given in ISO 13317-1 and the following apply. Stokes equivalent spherical diameter (m) (practical unit: micrometres,) Suspending liquid viscosity (), (practical unit:) Sedimentation
28、 height (m) Sample density effective particle density () Liquid density () Acceleration due to gravity () Sedimentation time, (seconds, s) Function of atomic number of sample elements in beam Concentration of sample in beam Attenuation of emergent X-ray beam passing through the suspending fluid Atte
29、nuation of emergent X-ray beam through suspension at settling height, at time X-ray density 5Sampling The sampling procedure according to ISO 13317-1 shall be followed. 6Representation of results The results shall be represented according to ISO 9276-1. 7Principle The concentration of dispersed samp
30、le is measured by attenuation of an X-ray beam. A stable, narrow, collimated beam of X-rays passes through a suspension of the sample: it is detected at a known height from the top of the sample cell. The sample cell is completely filled with sample suspension for the duration of the analysis. The s
31、ettling height, at which the particle concentration, is determined, may be reduced during the analysis for the purpose of obtaining a more rapid analysis than would be possible if all measurements were made at the same value of,. The cumulative mass percent of sample present at a given sedimentation
32、 height is continuously determined. The X- ray signal attenuation at the known height is compared to the attenuation with suspending liquid and also to the attenuation with the homogeneously dispersed sample present in the liquid. The attenuation of the emergent X-ray beam is proportional to the mas
33、s of powder in the beam, and is expressed by the following formula: (1) or (2) xStm PasmPas h skgm3 lkgm3 g9,807 ms2 t B C I0 Iht Dlg10(I0/I) hC h I = I0exp(BC) C = (1/B)ln(I/I0) Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical S
34、tandards 1/9972545001 Not for Resale, 04/21/2007 01:45:58 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 13317-3:2001(E) ISO 2001 All rights reserved 3 The X-ray density,is expressed as follows: (3) also (4) thus (5) The Stokes diameter, corresponding to the X-ray dens
35、ity at settling heightand time , is given by: (6) The X-ray densityis proportional to the concentration, and thus mass, of sample in the beam. A plot of the X- ray density, taken as a function of timeand, versus provides the cumulative mass distribution versus equivalent spherical diameter. 8Apparat
36、us 8.1Main apparatus The main apparatus (see Figure 1) typically consists of a temperature-controlled analysis compartment and mixing chamber; a plumbing system for circulation of suspending liquid or sample suspension; an X-ray source/detector system and a control module for apparatus control, data
37、 acquisition and reduction. The sedimentation cell within the temperature-regulated analysis compartment may be repositioned throughout the analysis relative to the signal source and detector to reduce analysis time. Alternative designs, such as one in which the X-ray source and detector move while
38、the sedimentation cell remains stationary, may also be used. The use of a magnetic stirrer should be avoided if magnetically susceptible particles are to be tested. The dispersion may then be maintained by means of a mechanical stirrer. 8.2Ancillary apparatus Ultrasonic bath, probe or high-speed mec
39、hanical stirrer capable of 500 revolutions to 1 000 revolutions per minute. D, D = BClge D =lg(I0/I) D = BClge=lg(I0/I) xStht xst= ? 18h (s l)gt ?1/2 DC Dth p 18h/(s l)gt Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards
40、 1/9972545001 Not for Resale, 04/21/2007 01:45:58 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 13317-3:2001(E) 4 ISO 2001 All rights reserved Figure 1 Schematic of typical apparatus using the X-ray gravitational technique Copyright International Organization for Stan
41、dardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/21/2007 01:45:58 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 13317-3:2001(E) ISO 2001 All rights reserved 5 9Sample preparation A representative samp
42、le for analysis shall be taken according to ISO 8213. It shall be dispersed according to ISO 14887 in a suspending medium of adequate viscosity and X-ray transparency. The use of dispersing agents and ultrasonics or mechanical stirring to aid dispersion will be recorded. Typicallyof dispersed sample
43、 is required for the analysis. The sample concentration will be prepared in accordance with the manufacturers instructions. Higher sample concentrations may be required with powders having a low X-ray absorptivity coefficient. Knowledge of the exact sample concentration is not required, but the infl
44、uence of concentration should be checked. The minimum concentration of suspension compatible with the measuring method is preferred (see ISO 13317-1). The required sample concentration will typically produce a reduction in the beam signal oftorelative to the signal observed with the suspending liqui
45、d. The sample may be dispersed in either an aqueous or an organic medium. Any liquid compatible with sample cell materials and having low absorptivity for X-rays may be used. Typical liquids are water, glycols, kerosene, mineral oils, alcohols and mineral spirits. It is recommended that the viscosit
46、y of the suspending medium should have a value such that the largest particle to be measured has a Reynolds number of(see ISO 13317-1). Any temperature change of the suspension should be minimized during a measurement (see 10.3). The viscosity and density of the suspending liquid at the temperature
47、of the analysis will be reported. The effective particle density of the sample is also reported. The suspending liquid, including dispersants at the analysis concentration, may be used as the displacement fluid to experimentally determine the effective particle density. 10Procedure 10.1General See I
48、SO 13317-1 for guidance on restrictions of upper size limit and lower size limit, and on test conditions. The validity of the measurement will be dependent on the Stokes equation applying to creeping flow for the suspension under study. The lower size limitation will in part be a function of the ability of the system to minimize thermal convection and mechanical effects. Additionally, for the fine size fraction, Brownian motion effects ma