1、 ISO 2017 Preparation of particulate reference materials Part 1: Polydisperse material based on picket fence of monodisperse spherical particles Prparation des matriaux de rfrence ltat particulaire Partie 1: Matriaux polydisperss composs dun ensemble de particules sphriques monodisperses TECHNICAL S
2、PECIFICATION ISO/TS 14411-1 Reference number ISO/TS 14411-1:2017(E) First edition 2017-05 ISO/TS 14411-1:2017(E)ii ISO 2017 All rights reserved COPYRIGHT PROTECTED DOCUMENT ISO 2017, Published in Switzerland All rights reserved. Unless otherwise specified, no part of this publication may be reproduc
3、ed or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requester. I
4、SO copyright office Ch. de Blandonnet 8 CP 401 CH-1214 Vernier, Geneva, Switzerland Tel. +41 22 749 01 11 Fax +41 22 749 09 47 copyrightiso.org www.iso.org ISO/TS 14411-1:2017(E)Foreword iv Introduction v 1 Scope . 1 2 Normative references 1 3 T erms, definitions and s ymbols 1 3.1 Terms and definit
5、ions . 1 3.2 Symbols . 2 4 Material requirements for preparing the individual monodisperse fractions .3 4.1 General description . 3 4.2 Requirements on the general properties of the material for individual pickets 3 5 Characterization of the individual monodisperse fractions . 4 5.1 Particle size di
6、stribution 4 5.2 Aspect ratio 5 5.3 Density . 5 5.4 Refractive index 5 6 Preparation of picket-fence distributions . 5 6.1 General . 5 6.2 Preparation of individual pickets 6 6.2.1 General 6 6.2.2 Preparation of suspensions from dry powders . 6 6.2.3 Determination of the particle mass fraction of su
7、spensions . 6 6.3 Preparation of a picket fence distribution. 6 6.3.1 General 6 6.3.2 Preparation from dry powders 6 6.3.3 Preparation from suspensions . 7 7 Estimation of uncertainties . 7 7.1 General . 7 7.2 Uncertainty of a volume-based size distribution due to limited number of particles counted
8、 . 7 7.3 Uncertainty of a number-based size distribution . 8 7.4 Picket-fence distributions composed of more than two kinds of quasi- monodisperse particles . 9 7.5 Uncertainty of a count base size distribution due to various number fraction .10 7.6 Uncertainty of a mass base size distribution due t
9、o various mass fractions .10 7.7 Uncertainty estimation based on the data before or after the mixing process 10 7.8 Uncertainty due to microscopic scale measurement 12 7.9 Uncertainty due to surrounding particles in microscopic measurement .12 7.10 Other uncertainty contributions 12 7.11 Combined un
10、certainty .12 Annex A (informative) Picket-fence distributions composed of more than two kinds of quasi-monodisperse particles .13 Annex B (informative) Example of reliability calculation for a mass-based cumulative size distribution transformed from the number-based size distribution .16 Annex C (i
11、nformative) Example of uncertainty estimation due to mixture fraction and sample size 19 Annex D (informative) Uncertainty estimation of various cases .21 Bibliography .28 ISO 2017 All rights reserved iii Contents Page ISO/TS 14411-1:2017(E) Foreword ISO (the International Organization for Standardi
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18、iso/ foreword .html. This document was prepared by Technical Committee TC 24, Particle characterization including sieving, Subcommittee SC 4, Particle characterization.iv ISO 2017 All rights reserved ISO/TS 14411-1:2017(E) Introduction The measurement of the particle size distribution can be accompl
19、ished by a number of techniques which measure some 1-D characteristic of the particle and usually equate this to an equivalent size assuming ideal shapes (usually spherical). Thus, these techniques usually require or assume knowledge of some other constant in order to calculate the particle size dis
20、tribution. Each of these techniques measures different properties which makes the equivalent particle size a method-defined measurand. Comparability of results therefore requires application of the same methods, which in turn requires standardization. This unsatisfactory situation of fundamental lac
21、k of comparability could be improved by a better understanding of the effects influencing the various methods. Since the sample material represents the link between the different methods, it is of central importance that it should meet as many physical assumptions of the considered methods as possib
22、le. A feasible approach is mixing known amounts of spherical, monodisperse particle fractions to create a polydisperse mixture (“picket fence distribution”). The individual particles should be spherical, as many sizing methods assume the particles to be spherical. Using particles that are in fact sp
23、herical fulfils this assumption, so the results of the various methods should be the same as far as the particle shape is concerned. A further advantage of spherical particles is that their size can be described by a single parameter only, the particle diameter. The individual fractions of the mixtu
24、re need to be monodisperse, as only then it is possible to trace the particle diameter back to the standard meter with an acceptable uncertainty and to get mixtures of theoretically known particle size distributions in the end. These materials should be used as follows. The monodisperse particle fra
25、ctions can be used to demonstrate equivalence of results with these ideal particles. If a method gives deviating results, the method is not yet fully understood and further investigation of the deviation is needed. The polydisperse mixtures can be used to challenge measurement methods to see what th
26、e output is. Final outcome should be a comprehensive understanding of the methods including particle dispersion, particle transport, physical principle and evaluation leading to better comparability of results. The approach described in this document is based on Reference 22 and Reference 23. A seco
27、nd approach is developing a theoretical framework for more accurate measurement of particle size distributions. Also, this approach is fundamentally limited to spherical particles of equal density, to be applicable to different methods. This document describes preparation protocols of picket fence d
28、istributions of spherical, quasi- monodisperse particulate reference materials. ISO 2017 All rights reserved v Preparation of particulate reference materials Part 1: Polydisperse material based on picket fence of monodisperse spherical particles 1 Scope This document describes the preparation of pol
29、ydisperse spherical particles based on a picket fence of quasi-monodisperse reference materials, the characterization of its monodisperse components with acceptable uncertainty and the estimation of the uncertainty of the mixture of these particles. This type of material is normally suitable for all
30、 particle characterization methods within the appropriate limits of the techniques. An example of using these reference materials in a reliability calculation for a mass-based cumulative size distribution is provided. This document limits itself to the technical specificities of preparation beyond t
31、he general requirements for certified and non-certified reference materials as described in ISO Guide 30, ISO Guide 31, ISO Guide 35 and ISO 17034. 2 Normative references There are no normative references in this document. 3 T erms, d efinitions and s ymbols 3.1 T erms and definiti ons For the purpo
32、ses of this document, the following terms and definitions apply. ISO and IEC maintain terminological databases for use in standardization at the following addresses: IEC Electropedia: available at h t t p :/ www .electropedia .org/ ISO Online browsing platform: available at h t t p :/ www .iso .org/
33、 obp 3.1.1 aspect ratio ratio of minimum Feret diameter to the maximum Feret diameter of a particle SOURCE: ISO 26824:2013, 4.5, modified 3.1.2 pycnometry method wherein particle density is obtained from the measured mass of sample with a given calibrated volume SOURCE: ISO 26824:2013, 2.4 TECHNICAL
34、 SPECIFICATION ISO/TS 14411-1:2017(E) ISO 2017 All rights reserved 1 ISO/TS 14411-1:2017(E) 3.1.3 apparent particle density particle mass in the dry status divided by the volume it would occupy including all pores, closed or open, and surface fissures SOURCE: ISO 13317-4:2014, 3.1 3.1.4 hydrostatic
35、balance method to measure particle density based on particle dynamic sedimentation velocity with known fluid density and viscosity condition 3.1.5 reference material material, sufficiently homogeneous and stable with respect to one or more specified properties, which has been established to be fit f
36、or its intended use in a measurement process SOURCE: ISO Guide 30:2015 3.1.6 c er t i f i e d r ef er en c e m a t er i a l reference material (3.1.5) characterized by a metrologically valid procedure for one or more specified properties, accompanied by a certificate that provides the value of the s
37、pecified property, its associated uncertainty, and a statement of metrological traceability SOURCE: ISO Guide 30:2015 3.1.7 nominal value designated diameter in terms of a target value in a given specification Note 1 to entry: The nominal value is the target diameter for an individual picket as calc
38、ulated from the upper and lower size of the picket fence distribution (3.1.8), the number of pickets and the requirement of equal spacing of pickets on a lognormal scale. Actual values may differ from the nominal ones due to the availability of suitable material 3.1.8 picket fence distribution mixtu
39、re of several monodisperse particle fractions (pickets) 3.2 Symbols Symbol Quantity Unit Derived unit i Particle mass fraction for the suspension of picket i kg/kg mg/kg i (0) Particle number fraction for the suspension of picket i x i Particle size interval in size range i m m Uncertainty of the pa
40、rameter given in the index NOTE: In other fields of measurement science and ISO/ IEC Guide 983 (GUM), the symbol u is used instead. x i Uncertainty of the size x i m m g Parameter defined by Formula (A.1) M Parameter used in Formula (A.5) m b Mass of the vessel for the dry mass determination kg mg m
41、 d Dry mass (vessel and particles) in the dry mass determination kg mg m i Mass of suspension i used for the preparation of the pick- et-fence distribution kg mg2 ISO 2017 All rights reserved ISO/TS 14411-1:2017(E) Symbol Quantity Unit Derived unit m l,i Mass of solvent of picket i kg mg m p,i Mass
42、of particles of picket i in suspension kg mg m s Mass of suspension used for the dry mass determination kg mg m x , i Mass of the particles of picket i in the final picket fence dis- tribution kg mg N, N i Total number of particles and particle number of picket i n i Number of particles in size rang
43、e i n picket Total number of pickets p Total number of uncertainty factors q 0 (x) Density distribution by number m 1 m 1 q 3 (x) Density distribution by volume or mass m 1 m 1 Q 0 (x) Cumulative distribution by number Q 0,i *,Q 3,i * True cumulative distribution by number and mass with logarithmic
44、abscissa Q 3 (x) Cumulative distribution by volume or mass i Particle density of picket i kg m 3 g cm 3 s Standard deviation of the particle size distribution m m s g Geometric standard deviation u Parameter used in Formula (6) to give confidence level, u = 1,96 for 95 % probability reliability NOTE
45、 This corresponds to the coverage factor k in ISO/ IEC Guide 983 (GUM). x ,x i Particle diameter and particle diameter in size range i m m x l Diameter of the smallest picket m m x u Diameter of the largest picket m m Median diameter of particle i based on number and mass m m x 50,3 Median particle
46、size of cumulative volume or mass distribu- tion m m x* 50,3 Most reliable median particle size of a cumulative volume or mass distribution with logarithmic abscissa m m 4 Material requirements for preparing the individual monodisperse fractions 4.1 General description The material of the individual
47、 pickets shall be suitable for particle size measurement using image analysis methods within dry or aqueous environment. 4.2 Requirements on the general properties of the material for individual pickets The material of the individual pickets shall meet the following requirements. a) The particles sh
48、all be spherical without significant macroscopic concavities, outgrowths or pores. The aspect ratio of all particles shall exceed a value of 0,95. A typical mean aspect ratio should be 0,97. Alternatively, the ellipse ratio shall exceed 0,95, a typical value should be 0,97 or above. ISO 2017 All rig
49、hts reserved 3 ISO/TS 14411-1:2017(E) b) When dispersed in pure water, no colour bleeding is allowed. The optical homogeneity of the material is very important to be as uniform as possible. This applies for the particles within one monodisperse fraction, as well as for a comparison of the particles of two different monodisperse fractions. c) The particle surface should be smooth without any contaminations or adhesions
