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1、BRITISH STANDARD BS ISO 13322-1:2004 Particle size analysis Image analysis methods Part 1: Static image analysis methods ICS 19.120 ? Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 04:34:05 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 13322-1:2004 This British Standard was published und
2、er the authority of the Standards Policy and Strategy Committee on 30 January 2006 BSI 30 January 2006 ISBN 0 580 47403 8 National foreword This British Standard reproduces verbatim ISO 13322-1:2004 and implements it as the UK national standard. The UK participation in its preparation was entrusted
3、to Technical Committee LBI/37, Sieves, screens and particle sizing, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international publications referred to in thi
4、s document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions of a con
5、tract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals
6、for change, and keep UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the ISO title page, pages ii to v, a blank page, pages 1 to 39 and a back cover. The BSI c
7、opyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 04:34:05 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Reference number ISO 13322-1:2004(E) INTERNATIO
8、NAL 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 BS ISO 13322-1:2004 Licensed Copy: sheffieldun sheffieldun, na, Sun
9、 Nov 26 04:34:05 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ii Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 04:34:05 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iii Contents Page Forewordiv Introduction v 1 Scope1 2 Normative references .1 3 Terms, abbreviated terms, definitions, and symbol
10、s1 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 instrument7 6 Microsco
11、py 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) Operating magnif
12、ication34 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 Bibliography .39 BS ISO
13、13322-1:2004 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 04:34:05 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iv Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International
14、 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-governmental, in liaison with ISO, a
15、lso 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, Part 2. The main task of technical commit
16、tees 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 casting a vote. Attention is drawn to the pos
17、sibility 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 13322-1 was prepared by Technical Committee ISO/TC 24, Sieves, sieving and other sizing methods, Subcommittee SC 4, Sizing by
18、methods other than sieving. ISO 13322 consists of the following parts, under the general title Particle size analysis Image analysis methods: Part 1: Static image analysis methods Part 2: Dynamic image analysis methods BS ISO 13322-1:2004 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 04:34:
19、05 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 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 a technique used in very different applications on image materia
20、l 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 description of the technique used and a standardized validation. This par
21、t 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, of known size so that the likely systematic uncertainties intro
22、duced 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 information is valid. Measurement of particle-size distributions by m
23、icroscopy 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 splitting the original sample and making measurements on three o
24、r 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 sample to generation of the final result add to the total uncertainty
25、 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 sample preparation expertise available, it is not intended to give a
26、 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. BS ISO 13322-1:2004 Licensed Copy: sheffieldun sheffieldun, na, Sun
27、 Nov 26 04:34:05 GMT+00:00 2006, Uncontrolled Copy, (c) BSI blank Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 04:34:05 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 1 Particle size analysis Image analysis methods Part 1: Static image analysis methods 1 Scope This part of ISO 13322 is applica
28、ble 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 as glass slides, stubs, filters, etc. Image analysis can recover particle images directly from microsco
29、pes 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 deviation of 1,6 of a log-normal distribution corresponds to a distribution of less than 10:1 in size. Suc
30、h 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 percentiles, at least 61 000 particles must be measured. This is described in Annex A. 2 Normative reference
31、s 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 referenced document (including any amendments) applies. ISO 9276-1, Representation of results of partic
32、le 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 size distributions 3 Terms, abbreviated terms, definitions and symbols 3.1 Terms, abbreviated terms and
33、 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 3.1.2 measurement frame field in a view field in which particles are counted for image analysis NOTE Th
34、e set of measurement frames composes the total measurement field. BS ISO 13322-1:2004 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 04:34:05 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 2 3.1.3 binary image digitized image consisting of an array of pixels, each of which has a value of 0 or 1,
35、 whose values are normally 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
36、inside the objects, which 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 ca
37、n have holes, the Euler 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
38、, i.e., 4-connectivity 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 Hayw
39、ood Diameter. 3.1.8 grey 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
40、 and the sine of the semi-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
41、 noun part into which something can be divided; subdivision or section 3.1.13 segmentation verb act of dividing something into segments BS ISO 13322-1:2004 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 04:34:05 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 3 3.1.14 threshold grey level value w
42、hich is set to discriminate objects of interest from background 3.2 Symbols error half-angle subtended by the particle at the objective lens wavelength, expressed in micrometres refractive index of the surrounding medium shape factor i A projected area of particle i d minimum feature length cal H ho
43、rizontal calibration factor K constant numerically determined by the confidence limit N number of particles to be measured i n numbers of particles 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 calibrati
44、on 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 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 d
45、iameter 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 upper limit of a class interval 1 X horizontal dimension of object BS ISO 13322-1:2004 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 04:34:05 GMT+
46、00:00 2006, Uncontrolled Copy, (c) BSI 4 X1,m horizontal dimension, expressed in micrometres X1,p horizontal dimension, expressed in pixels 2 X vertical dimension of object X2,m vertical dimension, expressed in micrometres X2,p vertical dimension, expressed in pixels 1 Z horizontal side length of th
47、e rectangular measurement frame 2 Z vertical side length of the rectangular measurement frame 4 Sample preparation demands for method description 4.1 General recommendations 4.1.1 General The following recommendations provide a sampling of standard microscopy practices. NOTE See References 4, 5 and
48、10 for additional suggestions. 4.1.2 Sample subdivision As only a small amount is needed to prepare a sample, the whole sample shall be subdivided in a manner that ensures that the portion taken is representative of the whole. The method used to subdivide the sample is likely to be dictated by the s
49、ample preparation method and will be decided by the laboratory performing the analysis. Provided that the sample is well dispersed by the method and that there is no segregation of particles by size, the choice of method is left to the expertise of the laboratory, since any specialized equipment required by a particular method might not be available to all. 4.1.3 Touching particles The number of particles touching each other should be minimized. It is a prime