ISO 13317-4:2014

Determination of particle size distribution by gravitational liquid sedimentation methods — Part 4: Balance method

ISO 13317-4:2014 specifies the method for the determination of particle size distribution by the mass of particles settling under gravity in liquid. This method is based on a direct mass measurement and gives the mass distribution of equivalent spherical particle diameter. Typically, the gravitational liquid sedimentation method applies to samples in the 1 μm to 100 μm size range and where the sedimentation condition for particle Reynolds number less than 0,25 is satisfied.

Détermination de la distribution granulométrique par les méthodes de sédimentation par gravité dans un liquide — Partie 4: Méthode de la balance

General Information

• Status: Published
• Publication Date: 13-Nov-2014
• ICS: 19.120 - Particle size analysis. Sieving
• Technical Committee: ISO/TC 24/SC 4 - Particle characterization
• Drafting Committee: ISO/TC 24/SC 4/WG 2 - Sedimentation, classification
• Current Stage: 9093 - International Standard confirmed
• Completion Date: 04-Mar-2020

Standards Content (Sample)

INTERNATIONAL ISO
STANDARD 13317-4
First edition
2014-11-15
Determination of particle size
distribution by gravitational liquid
sedimentation methods —
Part 4:
Balance method
Détermination de la distribution granulométrique par les méthodes
de sédimentation par gravité dans un liquide —
Partie 4: Méthode de la balance
Reference number
ISO 13317-4:2014(E)
©
ISO 2014

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ISO 13317-4:2014(E)

COPYRIGHT PROTECTED DOCUMENT
© ISO 2014
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
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Published in Switzerland
ii © ISO 2014 – All rights reserved

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ISO 13317-4:2014(E)

Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Symbols . 2
5 Principle of Method . 2
6 Measurement apparatus . 3
7 Measuring method . 4
7.1 Measurement of density . 4
7.2 Preparation method of suspension . 4
7.3 Measurement . 5
7.4 Data analysis . 6
8 Accuracy . 8
9 Size range of measurement . 8
10 Data representation . 8
Annex A (informative) Data reduction by matrix method .10
Bibliography .14
© ISO 2014 – All rights reserved iii

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ISO 13317-4:2014(E)

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 meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical Barriers
to Trade (TBT), see the following URL: Foreword — Supplementary information.
The committee responsible for this document is ISO/TC 24, Particle characterization including sieving,
Subcommittee SC 4, Particle characterization.
ISO 13317 consists of the following parts, under the general title Determination of particle size distribution
by gravitational liquid sedimentation methods:
— Part 1: General principles and guidelines
— Part 2: Fixed pipette method
— Part 3: X-ray gravitational technique
— Part 4: Balance method
iv © ISO 2014 – All rights reserved

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ISO 13317-4:2014(E)

Introduction
This document is a part of the ISO 13317 series. It describes a method to determine particle size
distribution by use of the mass of particles deposited at a balance. This method is based on a direct mass
measurement and gives immediately the mass-based distribution of particle diameter. This method
does not use any fitting parameters. The results obtained are Stokes diameters.
© ISO 2014 – All rights reserved v

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INTERNATIONAL STANDARD ISO 13317-4:2014(E)
Determination of particle size distribution by gravitational
liquid sedimentation methods —
Part 4:
Balance method
1 Scope
This part of ISO 13317 specifies the method for the determination of particle size distribution by the
mass of particles settling under gravity in liquid. This method is based on a direct mass measurement and
gives the mass distribution of equivalent spherical particle diameter. Typically, the gravitational liquid
sedimentation method applies to samples in the 1 μm to 100 μm size range and where the sedimentation
condition for particle Reynolds number less than 0,25 is satisfied.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. 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 particle size analysis — Part 1: Graphical representation
ISO 13317-1, Determination of particle size distribution by gravitational liquid sedimentation methods —
Part 1: General principles and guidelines
ISO 14887, Sample preparation — Dispersing procedures for powders in liquids
ISO 14488, Particulate materials — Sampling and sample splitting for the determination of particulate
properties
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 13317-1 and the following
apply.
3.1
apparent particle density
particle mass divided by the volume it would occupy including all internal pores
© ISO 2014 – All rights reserved 1

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ISO 13317-4:2014(E)

4 Symbols
For the purposes of this part of ISO 13317, the following symbols apply.
Quantity Symbol Unit Derivative Unit
Mass of dispersion medium m kg —
l
Maximum amount of sample same as the first line m kg —
s
-3
Apparent particle density ρ kg · m
s
-3
Liquid density ρ kg · m
l
Cumulative mass for particle diameter greater than x M kg
i i
Total mass of particles M kg
max
Sedimentation time for particle having a diameter x
i
t , t s —
i
and time, respectively
Particle diameter x m —
i
Liquid viscosity η Pa · s
Sedimentation distance h m
-2
Gravity acceleration g m · s
Cumulative distribution by mass for particle diameter x Q dimensionless —
i 3,i
Sedimentation mass at time t and t , respectively G , G kg —
i end ti end
Particle diameter corresponding to time t required to
x m —
move distance h
Maximum particle diameter x m —
max
-1
Sedimentation velocity v (x) m · s
Response function g (t,x) dimensionless —
-1
Distribution density by mass q (x) m
3
-1
Distribution density by mass at time t q (x) m
i 3,i
(k)
Parameter defined by Formula (A.6) γ dimensionless —
i
5 Principle of Method
This method is based on particle settling in a gravitational field and uniformly dispersed particles at
start (homogeneous technique). The relationship between settling velocity v, that means the time t
required to settle the distance h, is defined by the following formula according to Stokes law.
2
ρρ− gx
h ()
sl
v== (1)
t 18η
From Formula (1), the Stokes diameter x is directly obtained.
18ηh
x = (2)
ρρ− gt
()
sl
The above formulae can be applied for Reynolds numbers of sedimenting particles less than 0,25. The
determination of the particle size by gravitational sedimentation is a cumulative method (see ISO 13317-1).
In this case, the method determines the rate at which solid particles settle from the suspension in a
known volume of cylindrical vessel to a given distance. The mass of particles settled at time t is summed
up from the mass of all particles of a diameter greater than x and in part of particles of diameters less
than x. This method does not use any fitting parameters to obtain particle size distribution.
2 © ISO 2014 – All rights reserved

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ISO 13317-4:2014(E)

6 Measurement apparatus
a) Measurement apparatus to obtain the mass of the sediment
The apparatus measures continuously the increase of the mass of the particles sedimented out from
the suspension. The apparatus shown in Figure 1 a) typically consists of a sedimentation container
and mass measuring system (see Reference [2]). Figure 1 b) shows other type of sedimentation tray
(see Reference [3]). For the mass measurement apparatus (electronic balance), detection precision shall
be at least 1 % of the total mass of particles in the detection tray.
a) b)
Key
1 controller 7 main inlet pipe
2 stirrer 8 bypass
3 dispersion bath 9 sedimentation container
4 valve 10 detection tray
5 precision electronic balance 11 personal computer
6 glove box
Figure 1 — Measurement apparatus — Sedimentation balance for particles in liquid
b) Sedimentation bath
A typical sedimentation bath is shown in Figure 2. The detection tray has a cylindrical side wall and
the clearance between the side wall of the tray and sedimentation bath shall be large enough to avoid
interaction between them. Dimensions for the tray are shown in Figure 2. The following ratios should
apply:
— 08,/81< 2 22
— 04,/30<

12 12
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ISO 13317-4:2014(E)

Key
1 support wire
2 suspension
3 sedimentation bath
4 detection tray
h sedimentation distance
Figure 2 — Detection container
c) Dispersion bath
In the bath, the particles have to be dispersed before measurement and the dispersion state has to be
checked (see ISO 14887).
d) Measuring system
Figure 1 shows a schematic diagram of the measuring system. By use of a time-controlled valve (key
4), a precision electronic balance (key 5), and a personal computer (key 11), the cumulative mass of the
sediment on the tray is automatically recorded.
7 Measuring method
7.1 Measurement of density
The apparent particle density for the setting shall be measured (refer to ISO 13317-1:2001, 5.4).
7.2 Preparation method of suspension
A representative sample according to ISO 14488 shall be dispersed according to ISO 14887 in a dispersion
medium.
7.2.1 Dispersion medium
When the test particles are not well dispersed by the dispersion medium, it is necessary to use a suitable
dispersing agent. In this case, the dispersion medium should satisfy the following requirements.
a) Viscosity of the dispersion medium has to be in a suitable range regarding the sedimentation time.
4 © ISO 2014 – All rights reserved

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ISO 13317-4:2014
...

DRAFT INTERNATIONAL STANDARD ISO/DIS 13317-4
ISO/TC 24/SC 4 Secretariat: DIN
Voting begins on Voting terminates on

2013-02-16 2013-05-16
INTERNATIONAL ORGANIZATION FOR STANDARDIZATION  •  МЕЖДУНАРОДНАЯ ОРГАНИЗАЦИЯ ПО СТАНДАРТИЗАЦИИ  •  ORGANISATION INTERNATIONALE DE NORMALISATION


Determination of particle size distribution by gravitational liquid
sedimentation methods —
Part 4:
Balance method
Détermination de la distribution granulométrique par les méthodes de sédimentation par gravité dans un
liquide —
Partie 4: Méthode de la balance
ICS 19.120









To expedite distribution, this document is circulated as received from the committee
secretariat. ISO Central Secretariat work of editing and text composition will be undertaken at
publication stage.
Pour accélérer la distribution, le présent document est distribué tel qu'il est parvenu du
secrétariat du comité. Le travail de rédaction et de composition de texte sera effectué au
Secrétariat central de l'ISO au stade de publication.



THIS DOCUMENT IS A DRAFT CIRCULATED FOR COMMENT AND APPROVAL. IT IS THEREFORE SUBJECT TO CHANGE AND MAY NOT BE
REFERRED TO AS AN INTERNATIONAL STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS BEING ACCEPTABLE FOR INDUSTRIAL, TECHNOLOGICAL, COMMERCIAL AND USER PURPOSES, DRAFT
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RECIPIENTS OF THIS DRAFT ARE INVITED TO SUBMIT, WITH THEIR COMMENTS, NOTIFICATION OF ANY RELEVANT PATENT RIGHTS OF WHICH
THEY ARE AWARE AND TO PROVIDE SUPPORTING DOCUMENTATION.
©  International Organization for Standardization, 2013

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ISO/DIS 13317-4

Copyright notice
This ISO document is a Draft International Standard and is copyright-protected by ISO. Except as permitted
under the applicable laws of the user’s country, neither this ISO draft nor any extract from it may be
reproduced, stored in a retrieval system or transmitted in any form or by any means, electronic,
photocopying, recording or otherwise, without prior written permission being secured.
Requests for permission to reproduce should be addressed to either ISO at the address below or ISO’s
member body in the country of the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail [e-mail]
Web www.iso.org
Reproduction may be subject to royalty payments or a licensing agreement.
Violators may be prosecuted.

ii © ISO 2013 – All rights reserved

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ISO/DIS 13317-4

Contents Page
Foreword . iv
Introduction . v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Symbols . 2
5 Principle of Method . 2
6 Measuring apparatus . 2
7 Measuring method . 3
7.1 Measurement of density . 3
7.2 Preparation method of suspension . 3
7.2.1 Dispersion medium . 4
7.2.2 Suspension . 4
7.3 Measurement . 4
7.4 Data analysis . 5
7.4.1 Differential method . 5
7.4.2 Data reduction by matrix method . 6
8 Accuracy. 7
9 Reference materials . 7
10 Data representation . 8
Annex A (informative) Data reduction by matrix method . 9
A.1 Experimental conditions . 9
A.2 Data reduction by matrix method . 9
A.3 Example of measurement . 10
Bibliography . 13

© ISO 2012 – All rights reserved iii

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ISO/DIS 13317-4

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.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees 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 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.
ISO 13317-4 was prepared by Technical Committee ISO/TC 24, Particle characterization including sieving,
Subcommittee SC 4, Particle characterization.
ISO 13317 consists of the following parts, under the general title Determination of particle size distribution by
gravitational liquid sedimentation methods:
 Part 1: General principles and guidelines
 Part 2: Fixed pipette method
 Part 3: X-ray gravitational technique
 Part 4: Balance method
iv © ISO 2012 – All rights reserved

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ISO/DIS 13317-4

Introduction
This document is a part of ISO 13317 “Determination of particle size distributions by gravitational liquid
sedimentation methods”. It describes a method to determine particle size distribution by use of the mass of
particles deposited at a balance. This method is based on a direct mass measurement and gives immediately
the mass based distribution of particle diameter. This method does not use any fitting parameters. The results
obtained are Stokes diameters.

© ISO 2012 – All rights reserved v

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DRAFT INTERNATIONAL STANDARD ISO/DIS 13317-4

Determination of particle size distribution by gravitational liquid
sedimentation methods —
Part 4:
Balance method
1 Scope
This standard specifies the method for determination of particle size distribution by the mass of particles
settling under gravity in liquid. This method is based on a direct mass measurement and gives the mass
distribution of equivalent spherical particle diameter.
2 Normative references
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 particle size analysis — Part 1: Graphical representation
ISO 13317-1, Determination of particle size distribution by gravitational liquid sedimentation methods —
Part 1: General principles and guidelines
ISO 14887, Sample preparation-dispersing procedures of powders in liquids
ISO 14488, Particulate materials — Sampling and sample splitting for the determination of particulate
properties
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 13317-1 and the following apply.
3.1
Apparent particle density
particle mass divided by the volume it would occupy excluding all pores, and surface fissures (ISO 13317-1)








© ISO 2012 – All rights reserved
1

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ISO/DIS 13317-4

4 Symbols
For the purposes of this part of ISO 13317, the following symbols apply.
Quantity Symbol Unit Derivative Unit
Mass of dispersion medium m
kg —
l
Maximum amount of sample same as the first line m
kg —
s
-3
Apparent particle density ρ
kg · m
s
-3
Liquid density
ρ
kg · m
l
Cumulative mass for particle diameter greater than x M
kg
i i
Total mass of particles M
kg
max
Sedimentation time for particle having a diameter x
i
t , t
s —
i
and time, respectively
Particle diameter x
m —
i
Liquid viscosity kg/m/s Pa s
η
Sedimentation distance h m
-2
Gravity acceleration g
m · s
Cumulative distribution by mass for particle diameter x Q
dimensionless —
i 3,i
Sedimentation mass at time t and t , respectively G , G
kg —
i end ti end
Particle diameter corresponding to time t required to
x m —
move distance h

Maximum particle diameter x
m —
max
-1
Sedimentation velocity
v (x) m · s
Response function g (t,x) dimensionless —
-1
Distribution density by mass q (x)
m
3
-1
Distribution density by mass at time t q (x)

m
i 3,i
(k)
Parameter defined by Equation (A.6)
γ dimensionless —
i

5 Principle of Method
This method is based on particle settling in a gravitational field and uniformly dispersed particles at start
(homogeneous technique). The relationship between settling velocity v, that means the time t required to settle
the distance h, is defined by the following equation according to Stokes law.
2
(ρ − ρ )g x
h
s l
v = = (1)
t 18η
From equation (1) the Stokes equivalent spherical diameter x is directly obtained.
© ISO 2012 – All rights reserved
2

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ISO/DIS 13317-4

18η h
x = (2)
(ρ − ρ )g t
s l
The above equations can be applied for Reynolds numbers of sedimenting particles less than 0.25. The
determination of the particle size by gravitational sedimentation is a cumulative method (ISO 13317-1). In this
case the method determines the rate at which solid particles settle from the suspension in a known volume of
cylindrical vessel to a given distance. The mass of particles settled at time t is summed up from the mass of all
particles of a diameter greater than x and in part of particles of diameters less than x. This method does not
use any fitting parameters to obtain particle size distribution.
6 Measuring apparatus
a) Measuring apparatus to obtain the mass of the sediment
The apparatus measures continuously the increase of the mass of the particles sedimented out from the
suspension. The apparatus shown in Figure 1-(a) typically consists of a sedimentation container and mass
measuring system (ref. 2). Figure 1-(b) shows other type of sedimentation tray (ref. 3). For the mass
measuring apparatus (electronic balance) detection precision shall be at least 1 % of total mass of particles in
the detection tray.







a) b)
Key
1 Controller   7 Main inlet pipe
2 Stirrer   8 Bypass
3 Dispersion bath  9 Sedimentation container
4 Valve   10 Detection tray
5 Precision electronic balance 11 Personal computer
6 Glove box
Figure 1 — Measurement apparatus – sedimentation balance for particles in liquid
b) Sedimentation bath
A typical sedimentation bath is shown in Figure 2. The detection tray has a cylindrical side wall and the
clearance between the side wall of the tray and sedimentation bath shall be large enough to avoid interaction
between them. Dimensions for the tray are shown in Figure 2. The following ratios should apply:
© ISO 2012 – All rights reserved
2

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ISO/DIS 13317-4

h / d = 1.14, h / d = 1.48,
2 3 2
0.55 < d / d < 0.71, 0.78 < h / d < 0.90
1 2 1 2

Key
1 Support wire
2 Suspension
3 Sedimentation bath
4 Detection tray
h Sedimentation distance
Figure 2 — Detection container
c) Dispersion bath
In the bath the particles have to be dispersed before measurement and the dispersion state has to be checked
(see ISO 14887).
d) Measuring system
Figure 1 shows a schematic diagram of the measuring system. By use of a time controlled valve 4, a precision
electronic balance 5 and a personal computer 11, the cumulative mass of the sediment on the tray is
automatically recorded.
7 Measuring method
7.1 Measurement of density
The effective particle density shall be measured (refer to 5.4 of ISO 13317-1:2001).
7.2 Preparation method of suspension
A representative sample according to ISO 14488 shall be dispersed according to ISO 14887 in a dispersion
medium.
© ISO 2012 – All rights reserved
3

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