ISO/TS 14411-1:2017
(Main)Preparation of particulate reference materials — Part 1: Polydisperse material based on picket fence of monodisperse spherical particles
Preparation of particulate reference materials — Part 1: Polydisperse material based on picket fence of monodisperse spherical particles
ISO/TR 14411-1:2017 describes the preparation of polydisperse 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 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. ISO/TR 14411-1:2017 itself to the technical specificities of preparation beyond the general requirements for certified and non-certified reference materials as described in ISO Guide 30, ISO Guide 31, ISO Guide 35 and ISO 17034.
Préparation des matériaux de référence à l'état particulaire — Partie 1: Matériaux polydispersés composés d'un ensemble de particules sphériques monodispersées
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TECHNICAL ISO/TS
SPECIFICATION 14411-1
First edition
2017-05
Preparation of particulate reference
materials —
Part 1:
Polydisperse material based on picket
fence of monodisperse spherical
particles
Préparation des matériaux de référence à l’état particulaire —
Partie 1: Matériaux polydispersés composés d’un ensemble de
particules sphériques monodispersées
Reference number
©
ISO 2017
© ISO 2017, Published in Switzerland
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced 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 ISO’s member body in the country of
the requester.
ISO 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
copyright@iso.org
www.iso.org
ii © ISO 2017 – All rights reserved
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms, definitions and symbols . 1
3.1 Terms and definitions . 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 distribution . 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 suspensions . 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 . 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 to 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 uncertainty .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 (informative) Example of uncertainty estimation due to mixture fraction and
sample size .19
Annex D (informative) Uncertainty estimation of various cases .21
Bibliography .28
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 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) on all matters of
electrotechnical standardization.
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 documents 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).
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 responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www .iso .org/ patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO’s adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following
URL: w w w . i s o .org/ 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
Introduction
The measurement of the particle size distribution can be accomplished 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 distribution. 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 lack 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 possible. 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 spherical 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 mixture 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 fractions 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 the 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 second 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 distributions of spherical, quasi-
monodisperse particulate reference materials.
TECHNICAL SPECIFICATION ISO/TS 14411-1:2017(E)
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 polydisperse 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 particle
...
TECHNICAL ISO/TS
SPECIFICATION 14411-1
First edition
2017-05
Preparation of particulate reference
materials —
Part 1:
Polydisperse material based on picket
fence of monodisperse spherical
particles
Préparation des matériaux de référence à l’état particulaire —
Partie 1: Matériaux polydispersés composés d’un ensemble de
particules sphériques monodispersées
Reference number
©
ISO 2017
© ISO 2017, Published in Switzerland
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced 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 ISO’s member body in the country of
the requester.
ISO 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
copyright@iso.org
www.iso.org
ii © ISO 2017 – All rights reserved
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms, definitions and symbols . 1
3.1 Terms and definitions . 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 distribution . 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 suspensions . 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 . 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 to 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 uncertainty .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 (informative) Example of uncertainty estimation due to mixture fraction and
sample size .19
Annex D (informative) Uncertainty estimation of various cases .21
Bibliography .28
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 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) on all matters of
electrotechnical standardization.
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 documents 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).
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 responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www .iso .org/ patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO’s adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following
URL: w w w . i s o .org/ 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
Introduction
The measurement of the particle size distribution can be accomplished 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 distribution. 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 lack 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 possible. 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 spherical 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 mixture 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 fractions 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 the 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 second 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 distributions of spherical, quasi-
monodisperse particulate reference materials.
TECHNICAL SPECIFICATION ISO/TS 14411-1:2017(E)
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 polydisperse 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 particle
...
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