HORMUUD UNIVERSITY
Faculty of Engineering
Department of Chemical Engineering
Course Title: Particle
Technology
Chapter 02:
Characterization of
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Introduction
Particle properties such as particle shape and particle
density, together with the primary properties of a fluid
(viscosity and density), and also with the concentration and
state of dispersion, govern the secondary properties such
as settling velocity of particles, rehydration rate of powders,
resistance of filter cakes, and so on.
It could be argued that it is simpler, and more reliable, to
measure the secondary properties directly without
reference to the primary ones.
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Particle Size and Shape
The key characteristics of an individual particle include
composition, size, shape, density, and hardness
Composition determines properties such as density and
conductivity if the particle is uniform.
However, in many cases the particle is porous or it may
consist of a continuous matrix in which small particles of a
second material are distributed.
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Particle size is important because it affects properties
such as the surface per unit volume and the rate at which
a particle will settle in a fluid.
A particle shape may be regular, such as spherical or
cubic, or it may be irregular like a piece of broken glass.
Regular shapes can be defined by mathematical
equations, while irregular shapes and properties of
irregular particles are usually found by comparison to
specific characteristics of a regularly shaped particle.
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Single Particles
The simplest shape of a particle is the sphere. Because of
its symmetry, the particle looks exactly the same from
whatever direction it is viewed, and behaves in the same
manner in fluid, regardless of its orientation.
No other particle shape has this characteristic.
However, perfect spheres are rarely found and, generally, a
typical particle may not be of any regular known shape.
In fact, irregular-shaped particles are common.
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the size of a particle of an irregular shape is defined in
terms of the size of an equivalent sphere, although the
particle is represented by a sphere of a different size
according to the property that is selected.
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Some of the important sizes of equivalent spheres are
that the spheres have the same
1. volume as the particle.
2. surface area as the particle.
3. surface area per unit volume (i.e. specific surface area) as the particle.
4. area as the particle when projected onto a plane perpendicular to its
direction of motion.
5. projected area as the particle, as viewed from above, when lying in its
position of maximum stability such as on a microscope slide, for
example.
6. ability to pass through the same size of square aperture as the particle,
such as on a screen for example.
7. same settling velocity as the particle in a specified fluid.
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Several definitions depend on the measurement
of a particle in a particular orientation. Thus,
Feret’s statistical diameter is the mean
distance between two parallel lines that are
tangential to the particle in an arbitrarily fixed
direction, irrespective of the orientation of each
particle coming up for inspection. Similarly,
the Martin diameter is the length of the chord
that bisects the projected area of the particle.
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Both these diameters are shown in Fig. 2.1 for two
different orientations of the same particle.
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A measure of particle shape that is frequently
used is the sphericity, ψ, defined as:
where xp is the equivalent diameter of particle, sp is the
surface area of one particle, and Vp is the volume of one
particle.
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Other properties of the particle that may be important are
particle density, which can be crystalline, amorphous, or
porous, and the properties of its surface, which includes
roughness and presence of adsorbed films.
Particle hardness could also be important if the particle is
subject to heavy loading and/or impact.
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Measurement of Particle Size
Measurement of particle size and of particle size distribution is
a highly specialized topic, and considerable skill is needed to
make accurate measurements and interpretation.
Before a size analysis can be carried out, it is necessary to
collect a representative sample of the solids, and then reduce
this to the quantity, which is required for the chosen method of
analysis.
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Fig. 2.2
Sizes of typical
powder products.
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A wide range of measuring techniques is available for both
single particles and systems of particles, ranging from
• visual methods utilising microscopy and image analysis to
• stream or field scanning methods such as electronic
particle counters and laser diffractions.
In practice, each method is applicable to a finite range of sizes
and gives a particular equivalent size, dependent on the nature
of the method.
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Some Familiar Methods of Size Analysis
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Sieving (>50μm)
Sieve analysis may be carried
out using a nest of sieves, each
lower sieve being of smaller
aperture size.
Generally, sieve series is arranged so that the ratio of aperture sizes
on consecutive sieves is 2, , or according to the closeness of sizing
that is required.
The sieves may either be hand-shaken or mounted on a vibrator,
which should be designed to give a degree of vertical
movement and horizontal vibration.
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Whether or not a particle passes through an aperture
depends not only upon its size, but also on the probability
that it will be presented at the required orientation at the
surface of the screen.
The sizing is based purely on the linear dimensions of the
particle and the lower limit of size is determined by two
principal factors.
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First, the proportion of free space on the screen surface
becomes small as the size of the aperture is reduced.
Second, the attractive forces between particles become
larger at small particle sizes, and consequently particles tend
to stick together and block the screen.
Sieves are available in a number of standard series.
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There are several standard series of screens and the
sizes of the openings are determined by the thickness
of the wire used.
In the United Kingdom, British Standard (B.S.) screens
are made in sizes from 300-mesh and higher, although
they are too fragile for some work.
The Institute of Mining and Metallurgy (IMM) screens are
more robust, with the thickness of the wire approximately
equal to the size of the apertures.
The Tyler series, which is standard in the United States,
is intermediate, between the two British series.
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Table 2.1 Standard sieve sizes
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Screening may be carried out with either wet or dry
material.
In wet screening, material is washed evenly over the
screen and clogging is prevented.
In addition, small particles are washed off the surface of
large ones.
The obvious disadvantage is that it may be necessary to
dry the material afterwards.
With dry screening, the material is sometimes brushed
lightly over the screen to form a thin, even sheet.
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It is important that any agitation is not so vigorous that
size reduction occurs because screens are usually quite
fragile and are easily damaged by rough treatment.
In general, the larger and more abrasive the solids, the
more robust the screen should be.
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Cumulative Analysis
A second way to present the information is
through a cumulative analysis (Fig.) obtained by
adding the individual increments starting with
that containing the smallest particles, and
tabulating or plotting the cumulative sums
against the maximum particle diameter in the
increment
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The efficiency of screening is defined as the ratio of the
mass of material that passes the screen, to that which is
capable of passing through the screen.
This will differ according to the size of the material.
It may be assumed that the rate of passage of particles of a
given size through the screen is proportional to the number
or mass of particles of that size on the screen at any
instant. Thus, if w is the mass of particles of a particular
size on the screen at a time t, then:
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Thus, the mass of particles (w1-w2) passing the screen
in time t is given by
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It is important that any agitation is not so vigorous that size
reduction occurs because screens are usually quite fragile
and are easily damaged by rough treatment.
In general, the larger and more abrasive the solids, the
more robust the screen should be.
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Microscopic analysis (1–100μm)
Microscopic examination permits measurement of the
projected area of the particle and also enables an
assessment to be made of its two-dimensional shape.
In general, the third dimension cannot be determined
except when using special stereomicroscopes.
The apparent size of a particle is compared with that of
circles engraved on a graticule in the eyepiece
By using the electron microscope, the lower limit of size can
be reduced to about 0.001μm.
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Digital image processing
Advances in digital image capturing and image processing
make measurement of particle sizes relatively easy.
Commercial imaging setups utilising the image processing
techniques and providing reliable information about the
particle sizes are also available
The digital image of the particles is taken by a camera or
microscope and accurate results require the dispersal of the
particles in a non-touching fashion on a background having
good colour contrast.
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Often, instead of reporting this area, the equivalent diameter (
of the circle having area equal to the projected area of
particle is reported
Measurements for multiple particles can be done
simultaneously and the particle size distributions can be
easily obtained using this technique.
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Sedimentation and elutriation methods (>1μm)
These methods depend on the fact that the terminal
falling velocity of a particle in a fluid increases with size.
Sedimentation is the process of allowing particles in
suspension in water to settle out of the suspension
under the effect of gravity.
There are two main sedimentation methods.
1. the pipette method
2. the use of the sedimentation balance
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The elutriation method
is a reverse sedimentation process in which the particles
are dispersed in an upward flowing stream of fluid.
All particles with terminal falling velocities less than the
upward velocity of the fluid will be carried away.
A complete size analysis can be obtained by using
successively higher fluid velocities.
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Permeability methods (>1μm)
These methods depend on the fact that at low flow rates,
the flow rate through a packed bed is directly proportional
to the pressure difference, and the proportionality
constant being proportional to the square of the specific
surface (surface to volume ratio) of the powder.
From this method it is possible to obtain the diameter of
the sphere with the same specific surface as the powder.
The reliability of the method is dependent upon the care
with which the sample of powder is packed.
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Exercise
1. What does the shape of a particle affect?
2. What are the properties and characteristics of particulate solids?
3. Why is Particle Size Analysis Important?
4. Define sphericity.
5. Distinguish between differential and cumulative analysis.
6. Distinguish between Sedimentation and elutriation methods.
7. What are the key characteristics of an individual particle ?
8. How is the efficiency of screening defined?
9. What factors determine whether a particle passes through an aperture?
10. What is the elutriation method and how does it work?
11. What are some important sizes of equivalent spheres?
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