DULLIYAO, Van Vesper J.

Particle Technology

16-01480 Research Assignment

METHODS OF PARTICLE SIZE MEASUREMENT

I. Sieving (>45 μm)

For particle sizes greater than 45 μm, dry sieving using woven wire sieves is a simple and
cheap method of size analysis. Sieving gives a mass distribution and a size known as the sieve
diameter. Unless the particle is extremely elongated, the length of the particle does not hinder its
passage through the sieve apertures. The sieve diameter is then dependent on the maximum width
and maximum thickness of the particle. Sieve series are generally arranged so that the ratio of
aperture sizes on consecutive sieves is 2, 21/2 or 21/4 according to the closeness of sizing that is
required.

Figure 1 Log-normal distribution plotted on logarithmic coordinates

The sieves may either be hand shaken or mounted on a vibrator, the latter requiring to give
a degree of vertical movement in addition to the horizontal vibration. Size and the probability that
it will be presented at the required orientation at the surface of the screen decides whether or not a
particle passes through an aperture. The sizing is based purely on the linear dimensions of the
particle and the lower limit of size which can be used is determined by two principal factors. The
first is that the proportion of free space on the screen surface becomes very small as the size of the
aperture is reduced. The second is that 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. There are several standard series of screen and the sizes
of the openings are determined by the thickness of wire used.

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 The efficiency of screening is defined as the ratio of the mass of material which passes the
screen to that which is capable of passing. 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:
dw
 kw
dt
where k is a constant for a given size and shape of particle and for a given screen.
Thus, the mass of particles (w1 − w2) passing the screen in time t is given by:
w2
ln  kt
w1
If the screen contains a large proportion of material just a little larger than the maximum
size of particle which will pass, its capacity is considerably reduced. Screening is generally
continued either for a predetermined time or until the rate of screening falls off to a certain fixed
value.
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. This has the obvious disadvantage, however, that it may be necessary
to dry the material afterwards. With dry screening, the material is sometimes brushed lightly over
the screen so as to form a thin even sheet. It is important that any agitation is not so vigorous that
size reduction occurs, because screens are usually quite fragile and easily damaged by rough
treatment. In general, the larger and the more abrasive the solids the more robust is the screen
required.

II. Microscopy (1-100 μm)

Microscopic examination enables the measurement of projected area of a particle as well
the assessment to be made of its two-dimensional shape. The optical microscope may be used to
measure particle sizes down to 5 μm. For particles smaller than this diffraction causes the edges
of the particle to be blurred and this gives rise to an apparent size. The electron microscope may
be used for size analysis below 5 mm. Coupled with an image analysis system the optical
microscope or electron microscope can readily give number distributions of size and shape. Such

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systems calculate various diameters from the projected image of the particles (e.g. Martin’s,
Feret’s, shear, projected area diameters, etc.). Note that for irregular-shaped particles, the projected
area offered to the viewer can vary significantly depending on the orientation of the particle.
Techniques such as applying adhesive to the microscope slide may be used to ensure that the
particles are randomly orientated.

Figure 2 Particle profiles and comparison circles

III. Sedimentation (>1 μm)

This method is governed by the fact that the terminal velocity of a particle in a fluid
increases with size. The suspension is dilute and so the particles are assumed to fall at their single
particle terminal velocity in the liquid. Stokes’ law is assumed to apply (Rep < 0.3) and so the
method using water is suitable only for particles typically less than 50 μm in diameter. The rate of
sedimentation of the particles is followed by plotting the suspension density at a certain vertical
position against time. The suspension density is directly related to the cumulative undersize and
the time is related to the particle diameter via the terminal velocity. This is demonstrated in the
following:
Referring to Figure 2, the suspension density is sampled at a vertical distance, h below the
surface of the suspension. The following assumptions are made:
 The suspension is sufficiently dilute for the particles to settle as individuals (i.e.not
hindered settling).
 Motion of the particles in the liquid obeys Stokes’ law (true for particles typically smaller
than 50 μm).
 Particles are assumed to accelerate rapidly to their terminal free fall velocity UT so that the
time for acceleration is negligible.

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 Figure 3 Size Analysis by Sedimentation

Let the original uniform suspension density be C0. Let the suspension density at the sampling
point be C at time t after the start of settling. At time t all those particles travelling faster than h/t
will have fallen below the sampling point. The sample at time t will therefore consist only of
particles travelling a velocity ≤ h/t. Thus, if C0 is representative of the suspension density for the
whole population, then C represents the suspension density for all particles which travel at a
velocity ≤ h/t, and so C/C0 is the mass fraction of the original particles which travel at a velocity
≤ h/t. That is,
C
cumulative mass fraction =
C0
All particles travel at their terminal velocity given by Stokes’ law:
x 2 (ρ P  ρ f )g
UT 
18μ
Thus, equating UT with h/t, we determine the diameter of the particle travelling at our cut-off
velocity h/t. That is,
12
 18μ8 
x 
 t(ρ P  ρ f )g 

Particles smaller than x will travel slower than h/t and will still be in suspension at the sampling
point. Corresponding values of C/C0 and x therefore give us the cumulative mass distribution. The
particle size measured is the Stokes’ diameter, i.e. the diameter of a sphere having the same
terminal settling velocity in the Stokes region as the actual particle.

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Main Sedimentation Types
A. Pipette Method
At time intervals, samples are abstracted from the settling suspension at a fixed
horizontal level. Each sample contains a representative sample of the suspension, with the
exception of particles larger than a critical size, all of which will have settled below the level
of the sampling point. The most commonly used equipment, the Andreason pipette, is capable
of measuring 2-100 μm. At size below 2 μm, Brownian motion causes significant errors.
Increasing the body force acting on the particles by centrifuging the suspension permits the
effects of Brownian motion to be reduced so that particle sizes down to 0.01 μm can be
measured. The labour involved in this method may be reduced by using:
1. Light absorption method
The light absorption method gives rise to a distribution by surface.
2. X-ray absorption method
This method gives a mass distribution.
B. Hydrometer Method
The density of the suspension, which is related to the concentration, is read directly
from the stem of the hydrometer while the depth is determined by the distance of the
hydrometer bulb from the surface.
C. Gravitational Photo Sedimentation Methods
The change of the concentration with time and depth of sedimentation is monitored by
using a light point or line beam. These methods give a continuous record of changing optical
density with time and depth and have the added advantage that the beam can be scanned to the
surface to reduce the measurement time. A correction needs to be applied to compensate for a
deviation from the laws of geometric optics.
D. Gravitational X-ray Sedimentation Methods
The change of the concentration with time and depth of sedimentation is monitored by
using an X-ray beam. These methods give a continuous record of changing X-ray density with
time and depth and have the added advantage that the beam can be scanned to the surface to
reduce the measurement time. The methods are limited to materials having a high atomic mass
and give a distribution directly.

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 E. Sedimentation Balance Methods
Using a sedimentation balance, particles settle on an immersed balance pan which is continuously
weighed. The largest particles are deposited preferentially and consequently the rate of increase of
weight falls off progressively as particles settle out. The relationship between settled weight P,
weight undersize W, and time t is given by:
dP
P W 
d ln t
F. Centrifugal Sedimentation Methods
These methods extend sedimentation methods well into the submicrometer size range.
Alterations of the particle concentration may be determined space- and time-resolved during
centrifugation.

IV. Permeametry (>1 μm)

Permeability methods are size analysis dependent on fluid flow through a packed bed. At low
flowrates the flow through a packed bed is directly proportional to the pressure difference, the
proportionality constant being proportional to the square of the specific surface (surface: volume
ratio) of the powder.
The Carman–Kozeny equation for laminar flow through a randomly packed bed of
uniformly sized spheres of diameter is:
 Δp   180 1  ε 2  μU
H ε3 x2
where (-∆p) is the pressure drop across the bed, ε is the packed bed void fraction, H is the depth
of the bed, m is the fluid viscosity and U is the superficial fluid velocity. In dealing with non-
spherical particles with a distribution of sizes, the appropriate mean diameter for this equation is
the surface-volume diameter xSV, which may be calculated as the arithmetic mean of the surface
distribution, xaS.
In this method, the pressure gradient across a packed bed of known voidage is measured
as a function of flow rate. The diameter we calculate from the Carman–Kozeny equation is the
arithmetic mean of the surface distribution.

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 V. Electrozone Sensing
A well-diluted and -dispersed suspension in an electrolyte is caused to flow through a small
aperture. As the particles pass through, the changes in the resistivity between two electrodes
on either side of the aperture, are related to the volumes of the particles. The pulses are fed to
a pulse-height analyzer where they are counted and scaled. The method is limited by the
resolution of the pulse-height analyzer of about 16,000:1 (corresponding to a volume diameter
range of about 25:1) and the need to suspend the particles in an electrolyte. Although liquids
more viscous than water may be used to reduce sedimentation, the practical range of size for
this method is 0.3–1000 μm. Errors are introduced if more than one particle passes through the
orifice at a time and so dilute suspensions are used to reduce the likelihood of this error.

Figure 4 Schematic of electrozone sensing apparatus

VI. Laser Diffraction

This method relies on the fact that for light passing through a suspension, the diffraction
angle is inversely proportional to the particle size. An instrument would consist of a laser as a
source of coherent light of known fixed wavelength (typically 0.63 μm), a suitable detector
(usually a slice of photosensitive silicon with a number of discrete detectors, and some means of
passing the sample of particles through the laser light beam (techniques are available for
suspending particles in both liquids and gases are drawing them through the beam).
To relate diffraction angle with particle size, early instruments used the Fraunhofer theory,
which can give rise to large errors under some circumstances (e.g. when the refractive indices of
the particle material and suspending medium approach each other). Modern instruments use the

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Mie theory for interaction of light with matter. This allows particle sizing in the range 0.1–2000
μm, provided that the refractive indices of the particle material and suspending medium are known.
This method gives a volume distribution and measures a diameter known as the laser
diameter. Particle size analysis by laser diffraction is very common in industry today. The
associated software permits display of a variety of size distributions and means derived from the
original measured distribution.

References:
Green, D. W., & Perry, R. H. (2008). Perry's Chemical Engineering Handbook (8th ed.). The
McGraw-Hill Companies, Inc.

Rhodes, M. (2008). Introduction to Particle Technology (2nd ed.). England: John Wiley & Sons
Ltd.

Richardson, J., Harker, J., & Backhurst, J. (2002). Coulson and Richardson's CHEMICAL
ENGINEERING: Particle Technology and Separation Processes (5th ed., Vol. 2).
Butterworth Heinemann.