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1、 Reference number ISO 13322-1:2004(E) ISO 2004 INTERNATIONAL STANDARD ISO 13322-1 First edition 2004-12-01 Particle size analysis Image analysis methods Part 1: Static image analysis methods Analyse granulomtrique Mthodes par analyse dimages Partie 1: Mthodes par analyse dimages statiques Copyright
2、International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/07/2007 23:33:58 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 13322-1:2004(E) PDF disclaimer This PDF file may cont
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5、ameters were optimized for printing. 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. ISO 2004 All rights reserved. Unless otherw
6、ise 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
7、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 2004 All rights reserved Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technic
8、al Standards 1/9972545001 Not for Resale, 04/07/2007 23:33:58 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 13322-1:2004(E) ISO 2004 All rights reserved iii Contents Page Forewordiv Introduction v 1 Scope1 2 Normative references .1 3 Terms, abbreviated terms, definiti
9、ons, and symbols1 3.1 Terms, abbreviated terms and definitions1 3.2 Symbols .3 4 Sample preparation demands for method description.4 4.1 General recommendations.4 4.2 Suggested preparation methods.5 5 Image capture6 5.1 General.6 5.2 Procedures 7 5.3 Operating conditions for an image capture instrum
10、ent7 6 Microscopy and image analysis8 6.1 General.8 6.2 Size classes and magnification.9 6.3 Counting procedure9 7 Calculation of the particle size results .13 8 Test report13 Annex A (normative) Study on the sample size required for the estimation of mean particle diameter .15 Annex B (normative) O
11、perating magnification34 Annex C (normative) Resolution and sizing limits for typical objective lenses35 Annex D (informative) Flow chart showing a typical image analysis method .36 Annex E (informative) Statistical tests of mean and variance Analysis of variance and multiple comparisons37 Bibliogra
12、phy .39 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/07/2007 23:33:58 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 13322-1:2004(E) iv ISO 2004 All rig
13、hts 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 subject
14、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 (IEC) o
15、n all matters of electrotechnical standardization. International Standards are drafted in accordance 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
16、are circulated to the member bodies for voting. Publication as an International 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 document may be the subject of patent rights. ISO shall not be held
17、 responsible for identifying any or all such patent rights. ISO 13322-1 was prepared by Technical Committee ISO/TC 24, Sieves, sieving and other sizing methods, Subcommittee SC 4, Sizing by methods other than sieving. ISO 13322 consists of the following parts, under the general title Particle size a
18、nalysis Image analysis methods: Part 1: Static image analysis methods Part 2: Dynamic image analysis methods Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/07/2007 23:33:58 MDTNo reprod
19、uction or networking permitted without license from IHS -,-,- ISO 13322-1:2004(E) ISO 2004 All rights reserved v Introduction The purpose of this part of ISO 13322 is to give guidance for a measurement description and its validation when determining particle size by image analysis. Image analysis is
20、 a technique used in very different applications on image material with variations in material properties. Hence, it is not relevant to describe an exact standard method for determination of particle size by image analysis. The aim of this part of ISO 13322 is limited to give a standardized descript
21、ion of the technique used and a standardized validation. This part of ISO 13322 includes methods of calibration verification using a certified standard graticule as a reference or by using certified standard particles. It is sensible to make some measurements on particles, or other reference objects
22、, of known size so that the likely systematic uncertainties introduced by the equipment can be calculated. This part of ISO 13322 gives a recommendation for a precise description of the distribution including the number of analyzed particles and an analysis window to make sure that the obtained info
23、rmation is valid. Measurement of particle-size distributions by microscopy methods is apparently simple, but because only a small amount of sample is examined, considerable care has to be exercised in order to ensure that the analysis is representative of the bulk sample. This can be demonstrated by
24、 splitting the original sample and making measurements on three or more parts. Statistical analysis of the data, for example using the Students t-test, will reveal whether the samples are truly representative of the whole. Errors introduced at all stages of the analysis from sub-division of the samp
25、le to generation of the final result add to the total uncertainty of measurement and it is important to obtain estimates for the uncertainty arising from each stage. Indications where this is required are given at the appropriate point in the method. Because of the diverse range of equipment and sam
26、ple preparation expertise available, it is not intended to give a prescriptive procedure where use of individual methods does not jeopardize the validity of the data. However, essential operations are identified to ensure that measurements made conform to this part of ISO 13322 and are traceable. Co
27、pyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/07/2007 23:33:58 MDTNo reproduction or networking permitted without license from IHS -,-,- Copyright International Organization for Standard
28、ization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/07/2007 23:33:58 MDTNo reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARD ISO 13322-1:2004(E) ISO 2004 All rights reserved 1 Particle size analysis
29、 Image analysis methods Part 1: Static image analysis methods 1 Scope This part of ISO 13322 is applicable to the analysis of images for the purpose of determining particle size distributions. The particles are appropriately dispersed and fixed on an optical or electron microscope sample stage such
30、as glass slides, stubs, filters, etc. Image analysis can recover particle images directly from microscopes or from photomicrographs. Even though automation of the analysis is possible, this technique is basically limited to narrow size distributions of less than an order of magnitude. A standard dev
31、iation of 1,6 of a log-normal distribution corresponds to a distribution of less than 10:1 in size. Such a narrow distribution requires that over 6 000 particles be measured in order to obtain a repeatable volume-mean diameter. If reliable values are required for percentiles, e.g. D90 or other perce
32、ntiles, at least 61 000 particles must be measured. This is described in Annex A. 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
33、referenced document (including any amendments) applies. ISO 9276-1, Representation of results of particle size analysis Part 1: Graphical representation ISO 9276-2, Representation of results of particle size analysis Part 2: Calculations of average particle sizes/diameters and moments from particle
34、size distributions 3 Terms, abbreviated terms, definitions and symbols 3.1 Terms, abbreviated terms and definitions For the purposes of this document, the following definitions apply. 3.1.1 view field field which is viewed by a viewing device, e.g. optical microscope or electron scanning microscope
35、3.1.2 measurement frame field in a view field in which particles are counted for image analysis NOTE The set of measurement frames composes the total measurement field. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1
36、/9972545001 Not for Resale, 04/07/2007 23:33:58 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 13322-1:2004(E) 2 ISO 2004 All rights reserved 3.1.3 binary image digitized image consisting of an array of pixels, each of which has a value of 0 or 1, whose values are norm
37、ally represented by dark and bright regions on the display screen or by the use of two distinct colours 3.1.4 edge finding one of many edge detection methods used to detect transition between objects and background 3.1.5 Euler number number of objects minus the number of holes inside the objects, wh
38、ich describes the connectedness of a region, not its shape NOTE A connected region is one in which all pairs of points can be connected by a curve lying entirely in the region. If a complex two-dimensional object is considered to be a set of connected regions, where each one can have holes, the Eule
39、r number for such an object is defined as the number of connected regions minus the number of holes. The number of holes is one less than the connected regions in the set compliment of the object. It is important to report the Euler number together with the connectivity applied, i.e., 4-connectivity
40、 or 8-connectivity. 3.1.6 Feret diameter distance between two parallel tangents on opposite sides of the image of a particle 3.1.7 equivalent circular diameter ecd diameter of a circle having the same area as the projected image of the particle NOTE It is also known as the Haywood Diameter. 3.1.8 gr
41、ey image image in which multiple grey level values are permitted for each pixel 3.1.9 image analysis processing and data reduction operation which yields a numerical or logical result from an image 3.1.10 numerical aperture NA product of the refractive index of the object space and the sine of the s
42、emi-aperture of the cone of rays entering the entrance pupil of the objective lens from the object point 3.1.11 pixel picture element individual sample in a digital image that has been formed by uniform sampling in both the horizontal and vertical directions 3.1.12 segmentation noun part into which
43、something can be divided; subdivision or section 3.1.13 segmentation verb act of dividing something into segments Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/07/2007 23:33:58 MDTNo r
44、eproduction or networking permitted without license from IHS -,-,- ISO 13322-1:2004(E) ISO 2004 All rights reserved 3 3.1.14 threshold grey level value which is set to discriminate objects of interest from background 3.2 Symbols error half-angle subtended by the particle at the objective lens wavele
45、ngth, expressed in micrometres refractive index of the surrounding medium shape factor i A projected area of particle i d minimum feature length cal H horizontal calibration factor K constant numerically determined by the confidence limit N number of particles to be measured i n numbers of particles
46、 of size i X P probability i P probability that particle i exists in the measurement frame (also called Miles-Lantuejoul factor) cal V vertical calibration factor i V relative volume of particle i A X diameter of spherical particle i Ai X area equivalent diameter of particle i F1 X horizontal Feret
47、diameter of object F2 X vertical Feret diameter of object i X dimension of particle i maxi X longest dimension of particle i, also called maximum Feret diameter mini X shortest dimension of particle i, also called minimum Feret diameter XLIL lower limit of a class interval mean X mean of i X XUIL up
48、per limit of a class interval 1 X horizontal dimension of object Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/07/2007 23:33:58 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 13322-1:2004(E) 4 ISO 2004 All rights reserved X1,m horizontal dimension, expressed in microm