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









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©  International Organization for Standardization, 2013

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ISO/DIS 13317-4

Copyright notice
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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

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ISO/DIS 13317-4

Foreword
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(ISO member bodies). The work of preparing International Standards is normally carried out through ISO
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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
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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.

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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)








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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.
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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:
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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.
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