Determination of particle size distribution by gravitational liquid sedimentation methods — Part 5: Photosedimentation techniques

This document specifies principles and methods for the use of gravitational photosedimentation techniques for the characterization of dispersed phases of suspensions and emulsions. These techniques monitor the gravity-induced phase separation of particulate materials dispersed in liquids by recording photometric signals (i.e. intensity of transmitted or scattered light) as a function of either vertical position or measurement time, or both. This document does not cover particle migration by centrifugal, electric or magnetic forces, or sedimentation at high particle concentrations (e.g. zone sedimentation). Moreover, it does not cover the determination of properties other than sedimentation velocity and particle size (i.e. it does not cover particle concentration, particle shape, particle density, zeta-potential or apparent viscosity). Additionally, this document does not cover alternative techniques for gravitational sedimentation including balance based and X-ray based techniques. NOTE This document does not purport to address all the safety problems associated with its use.

Détermination de la distribution granulométrique par les méthodes de sédimentation par gravité dans un liquide — Partie 5: Techniques de photosédimentation

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Status
Published
Publication Date
12-Jan-2025
Current Stage
6060 - International Standard published
Start Date
13-Jan-2025
Due Date
13-Jan-2025
Completion Date
13-Jan-2025
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ISO 13317-5:2025 - Determination of particle size distribution by gravitational liquid sedimentation methods — Part 5: Photosedimentation techniques Released:13. 01. 2025
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International
Standard
ISO 13317-5
First edition
Determination of particle size
2025-01
distribution by gravitational liquid
sedimentation methods —
Part 5:
Photosedimentation techniques
Détermination de la distribution granulométrique par les
méthodes de sédimentation par gravité dans un liquide —
Partie 5: Techniques de photosédimentation
Reference number
© ISO 2025
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Published in Switzerland
ii
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Symbols and abbreviated terms. 6
5 Measurement principle and instrumentation . 8
5.1 General measurement principle .8
5.2 Primary and derived measurement results .10
5.3 Instrumentation .11
6 Measurement data and calculation of distribution function .13
6.1 Primary and derived measurands . 13
6.2 Intrinsically measured distribution functions . 15
6.3 Conversion to volume-weighted distribution functions .17
6.4 Determination of the start position .18
6.5 Assumptions behind data analysis in photosedimentation . 20
6.5.1 Assumptions related to Stokes law . 20
6.5.2 Assumptions related to photometric particle quantification .21
6.6 Working range with respect to particle size and concentration .21
6.6.1 Limits defined by the applicability of Stokes law .21
6.6.2 Limits defined by the applicability of photometric detection . 22
7 Performing size analyses .24
7.1 General .24
7.2 Sampling .24
7.3 Dispersion process and primary sample preparation.24
7.4 Secondary sample preparation (sample conditioning) . 25
7.5 Instrument preparation . 25
7.6 Measurement . 26
7.7 Data analysis . 26
7.8 Reporting .27
8 System qualification and quality control .28
8.1 General remarks . 28
8.2 Reference materials . 29
8.3 Performance qualification. 30
8.4 Measurement uncertainty . 30
Annex A (informative) Measurement position .33
Annex B (informative) Calculation of number-weighted particle size distribution .37
Annex C (informative) Detailed multi-wavelength approach .40
Annex D (informative) Guide to uncertainty determination .42
Annex E (informative) Beyond velocity and size determination. 47
Bibliography .50

iii
Foreword
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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).
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This document was prepared by Technical Committee ISO/TC 24, Particle characterization including sieving,
Subcommittee SC 4, Particle characterization.
A list of all parts in the ISO 13317 series can be found on the ISO website.
Any feedback or questions on this document should be directed to the user’s national standards body. A
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iv
Introduction
The principles of gravitational photosedimentation and its potential use for the granulometric
characterization of particle systems have been known for several decades. Recent developments in
optoelectronics and data processing have boosted the commercial success and popularity of this
measurement technique, which is currently employed in manifold academic and industrial applications.
This document is a part of the ISO 13317 series that provides a general overview on the principles, techniques,
methods and underlying physics of particle size analysis by gravitational sedimentation. Photosedimentation
employs photometric signals (i.e. transmitted, reflected or scattered light) in order to monitor the changes
in the local particle concentration, which arise by the downward or upward particle migration under
gravity (called hereafter sedimentation). The temporal or spatial functions of these signals can be directly
transformed to distributions of the sedimentation velocity, without referring to model assumptions or being
restricted by essential preconditions. Provided the applicability of Stokes’ law on particle mobility, one can
derive equivalent diameters from the sedimentation velocities (the Stokes diameter) and the corresponding
particle size distributions. Size fractions are then intrinsically weighted by photometric quantities (e.g. light
extinction or scattered light intensity), which is in contrast to the sedimentation techniques described in
ISO 13317-2, ISO 13317-3 and ISO 13317-4. However, conversion into volume-weighted distributions is often
an integrated part of signal processing, which employs established models for light-particle interactions. A
noteworthy feature of gravitational photosedimentation is its ability to finely resolve details in the particle
distribution functions. This is related to the physical fractionating of particle systems under gravity and
constitutes an advantage compared to spectroscopic ensemble techniques.
Gravitational photosedimentation facilitates the granulometric characterization of dispersed materials
of non-zero density contrast to the continuous phase, including solid particles and emulsion droplets.
The available measurement range depends on dispersed and continuous phase properties and typically
amounts to 200 nm to 100 μm for aqueous samples, whereas the sedimentation velocity can be quantified
for the range 0,6 µm/s to 10 mm/s. Also, the working range with regard to particle concentration is strongly
affected by material properties and by particle size, yet it is typically well below 1 vol%. The data analysis
relies on the assumption that all particles have the same density and comparable shape and do not undergo
chemical or physical change in the continuous phase.
In addition, photosedimentation techniques that monitor gravity-induced concentration changes along the
complete sample height, e.g. by position-scanning or time-resolved projection, facilitate the characterization
of dense dispersion beyond particle size, e.g. with respect to clarification, segregation, agglomeration,
consolidation and physico-chemical stability (see ISO/TR 13097). Gravitational photosed
...

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