Determination of particle size distribution by centrifugal liquid sedimentation methods — Part 1: General principles, requirements and guidance

This document specifies the principles of particle size analysis by centrifugal liquid sedimentation (CLS). It also: — defines the relevant terms; — describes the various measurement techniques; — gives guidance for sample preparation, conducting measurements as well as data analysis; — establishes rules for method validation, determination of the uncertainty budget as well as representation of results. An important part of this document deals with the derivation of particle size distributions from CLS data, including discussions on: — the impact of Brownian motion; — the parallel determination of particle concentrations; — the working range with respect to size and concentration; —the handling of non-spherical and porous particles. This document applies to samples composed of dispersions of low particle concentration, so that the particles’ motion can be considered as that of fully isolated particles. This document does not cover particle migration by gravity, electric or magnetic forces. It also does not cover deriving particle properties other than size, sedimentation velocity and sedimentation coefficient. NOTE This document can involve hazardous materials, operations and equipment. It does not purport to address all the safety problems associated with its use. Regulations regarding explosion-proof analysers can apply when examining volatile liquids with a low flash point. It is the responsibility of the user of this document to establish appropriate safety and health practices and to determine the applicability of the regulatory limitations prior to its use.

Détermination de la distribution granulométrique par les méthodes de sédimentation centrifuge dans un liquide — Partie 1: Principes généraux, exigences et orientation

General Information

Status
Published
Publication Date
30-Sep-2024
Current Stage
6060 - International Standard published
Start Date
01-Oct-2024
Due Date
18-Jan-2024
Completion Date
01-Oct-2024
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ISO 13318-1:2024 - Determination of particle size distribution by centrifugal liquid sedimentation methods — Part 1: General principles, requirements and guidance Released:1. 10. 2024
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International
Standard
ISO 13318-1
Second edition
Determination of particle size
2024-10
distribution by centrifugal liquid
sedimentation methods —
Part 1:
General principles, requirements
and guidance
Détermination de la distribution granulométrique par les
méthodes de sédimentation centrifuge dans un liquide —
Partie 1: Principes généraux, exigences et orientation
Reference number
© ISO 2024
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
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Published in Switzerland
ii
Contents Page
Foreword .v
Introduction .vi
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Symbols and abbreviated terms. 7
5 Measurement principle and technical realisations . 10
5.1 General measurement principle .10
5.2 Technical realisation of sedimentation-based centrifugal measurement techniques . 13
6 Measurement data and basic rules of data evaluation.15
6.1 Primary and derived measurands in centrifugal liquid sedimentation . 15
6.2 Spatial distribution of particles in centrifugal fields .17
6.3 Determination of distribution functions .18
6.3.1 General remarks .18
6.3.2 Distribution analysis for incremental techniques —homogeneous-start method
(HSM) .19
6.3.3 Distribution analysis for incremental techniques — line-start method (LSM) . 20
6.3.4 Distribution analysis for integral techniques .21
6.3.5 Conversion with respect to the type of quantity .21
6.3.6 Total quantity of dispersed phase and non-normalised particle size distributions . 22
6.3.7 Measurement analysis with respect to sedimentation and diffusion . 23
6.4 Deviations from Stokes-based analysis . 25
6.4.1 General . 25
6.4.2 Upper limit for sedimentation velocity and particle size . 25
6.4.3 Lower limits for particle size . 26
6.4.4 Limits for particle concentration .27
6.4.5 Handling of porous and heterogeneous particles .27
6.4.6 Handling of non-spherical particles and particle agglomerates .27
7 Performing size analyses .28
7.1 General . 28
7.2 Sampling . 28
7.3 Continuous phase and primary sample preparation . 28
7.4 Secondary sample preparation (sample conditioning) . 29
7.5 Instrument preparation . 30
7.6 Measurement . 30
7.6.1 General procedures for CLS . 30
7.6.2 Procedures for homogeneous-start method (HSM) .31
7.6.3 Procedures for line-start method (LSM) .31
7.6.4 Criteria for adjusting the rotational speed .32
7.7 Data analysis .32
7.8 Reporting . 33
8 System qualification and quality control .34
8.1 General remarks . 34
8.2 Reference materials . 35
8.3 Installation, operational and performance qualifications . 36
8.4 Sources of measurement uncertainty . 36
8.5 Accuracy and measurement of uncertainty of particle velocity and particle size . 38
8.6 Combined and expanded uncertainty of particle velocity and particle size measurement
(Stokes diameter) . 38
Annex A (informative) Particle sizing techniques based on centrifugal liquid sedimentation
(CLS) . 41

iii
Annex B (informative) Remarks on particle density .44
Annex C (informative) Sedimentation beyond the validity of Stokes’ law .50
Annex D (informative) Trueness, reproducibility and uncertainty determination for velocity
and particle size .57
Annex E (informative) Multiwavelength approach .62
Annex F (informative) Spatial distribution of particles in centrifugal fields .64
Annex G (informative) Additional particle and dispersion characteristics based on centrifugal
sedimentation velocity and sedimentation coefficient .73
Bibliography . 74

iv
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
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The procedures used to develop this document and those intended for its further maintenance are described
in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the different types
of ISO document should be noted. This document was drafted in accordance with the editorial rules of the
ISO/IEC Directives, Part 2 (see www.iso.org/directives).
ISO draws attention to the possibility that the implementation of this document may involve the use of (a)
patent(s). ISO takes no position concerning the evidence, validity or applicability of any claimed patent
rights in respect thereof. As of the date of publication of this document, ISO had not received notice of (a)
patent(s) which may be required to implement this document. However, implementers are cautioned that
this may not represent the latest information, which may be obtained from the patent database available at
www.iso.org/patents. ISO shall not be held responsible for identifying any or all such patent rights.
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This document was prepared by Technical Committee ISO/TC 24, Particle characterization including sieving,
Subcommittee SC 4, Particle characterization.
This second edition cancels and replaces the first edition (ISO 13318-1:2001), which has been technically
revised.
The main changes are as follows:
— revision of core terms (3.3, 3.5, 3.10, 3.11, 3.16, 3.14) and inclusion of further terms;
— revised and expanded explanation of measurement principle and techniques (Clauses 5 and 6);
— inclusion of the terminal sedimentation velocity as a measurand;
— introduction of informative annexes that provide:
— an overview of particle sizing techniques based on centrifugal liquid sedimentation (Annex A);
— remarks on particle density (Annex B);
— information regarding sedimentation beyond the validity of Stokes' law (Annex C);
— trueness, reproducibility and uncertainty determination for velocity and particle size (Annex D);
— an explanation on the mul
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