CHAPTER 2 : Characterization Particle

sizing
2.0 PARTICLE SIZE CHARACTERIZATION

2.1 Introduction to Particle Size and Shape

In many powder handling and processing

operations, particle size and size distribution
play a key role in determining the bulk
properties of the powder.

Example of regular-shaped particles.

Shape Dimensions
Sphere Radius
Cube Side length
Cylinder Radius and height
Cuboid Three side lengths
Cone Radius and height

In practice, it is important to use the method of

size measurement, which directly gives the
particle size, which is relevant to the situation, or
process of interest.
Methods of
measurement
1) Laser diffraction

Light passing through a suspension

Diffraction angle is inversely proportional
to the particle size
An instrument would consist of a laser
source and detector
Diffraction angle relate with particle
sizing- Farunhaufer theory and Mie
theory.
This method give volume dsitribution
Methods of
measurement
2) Electrozone sensing

Particle in suspension in a dilute

electrolyte which is drawn through a tiny
orifice with a voltage applied across it
As particles flow through the orifice a
voltage pulse is recorded
The amplitude of the pulse can be
related to the volume of the particle
passing the orifice
It will give a number of distribution of
the equivalent volume sphere diameter
Can detect 0.3-1000 mm
Methods of
measurement
3) Sieve

Dry sieving using woven wire sieves is a

simple and cheap method for particles
size greater than 45mm.
It givess mass distribution and a size
known as sieve diameter
Sieve diameer is dependant on the
maximum width and maximum thickness
of the particle.
If standard procedures are followed and
care is taken, sieving gives reliable and
reproducible analysis
Methods of
measurement
4) Sedimentation

The rate of sedimentation of particles in

liquid is followed
Suspension is dilute and the particles are
assumed to fall at their single particle
terminal velocity in the liquid
Stokes law is assumed to appy (Re<0.3)
Method using water is suitable for
particles less than 50 mm
Refer to section 1.8.3 (text book)
Methods of measurement
5) Microscopy

Optical microscopy can be used to measure particle sizes down to

5mm.
Coupled with image analysis, the optical microscope or electrone
microscope can readily give number distributions of size and
shape. Various diameters can be calculated from the projected
images (Martins, Ferets, shear, projected area)
2.2 Sampling method

Most laboratory tests use only a small sample

and this has to be taken from a production
stream or from an existing, stored material. This
sample has to be the representative of the
whole material.

Powders are unlike fluid where the properties

change easily under applied load.

They may consolidate with time, and attrition

and segregation may occur in transfer.

Sampling is an important element of powder

handling such that it demands careful scientific
design and operation of the sampling system.
 The purpose is to collect a manageable mass of
material (=sample), which is representative of
the total mass of powder from which it was
taken.

This is achieved by taking many small samples

from all parts of total which, when combined, will
represent the total with an acceptable degree of
accuracy.

This means that all particles in the total must

have the same probability of being included in
the final sample.
 To satisfy the above requirements, the following
basic golden rules of sampling should be
followed wherever practicable.

o Sampling should be made preferably from a

moving stream (this applies to both powders
and suspensions) but powder on a stopped
belt also can be sampled.

o A sample of the whole of the stream should

be taken for many (equal-spaced) periods of
time rather than part of the stream for the
whole of the time.

Re-combined primary sample taken from the

whole is too large for most powder test and so
that, it need to be sub-divided into secondary
or tertiary sub-sample.
 Allen (1981) reviewed and tested most
methods available for sampling splitting and
found the best is equipment called spinning
riffler (Figure 1).

In spinning riffler, the sample is slowly

conveyed by a vibratory feeder from the feed
hopper to the rotating carousel where it is
divided into many container ports via a
machined rotary head.

The sub-samples are collected in this

depending on how many samples are required.

Feed rate is controlled by varying the gap

under the hopper and varying the vibration of
the feeder.
2.3 Types Of Particle Diameters, Mean Size And
Size Distribution.

2.3.1 Types of particle diameters

Some definitions of terms used:

dp = Sieve size, the width of the minimum

square aperture through which the
particle will pass

dv = Volume diameter, the diameter of a

sphere having the same volume as the
particle.

dsv = Surface/volume diameter, the diameter

of a sphere having the same external
surface area/volume ratio as the
particle.

ds = Surface diameter, the diameter of a

sphere having the same surface as the
particle.
 Some of the diameters are related through
Waddells sphericity factor, , defined as;

= surface area of equivalent volume sphere

surface area of the particle

Some common diameters used in microscopy

analysis are:
Equivalent circle diameter
Martins diameter
Ferret diameter
Shear diameter
2
d
v (2.1)
ds
d
or sv (2.2)
dv

, dv and dsv can be calculated exactly for

geometrical shapes such as cuboids, rings etc.
 According to Geldart (1989), in practice, value of
for a specific material can be obtained as
follows;

o Sieve out a narrow size fraction of the

powder, usually the middle of the size range
or the coarser material, so as to obtain at
least 0.5 1 kg.

o Split this down using a riffler to obtain a few

hundreds particles.

o Count the exact number (n) and weight

them (M). Knowing the particle density, p,
calculate the equivalent sphere volume
diameter, dv from

1/ 3
6M
dv

p
n (2.3)
o Put the 0.5 1 kg of powder in a circular
tube 50 75 mm diameter and measure the
pressure drop, P, across the bed at a
variety of low flowrates.

o The Carman-Kozeny equation relates

pressure drop to particle size, dsv, voidage
and bed depth, L at low Reynolds number.

P 1501 mU
2

(2.4)
L 3 d sv2

o Thus, dsv can be calculated from pressure

drop data.

o From equation above, calculate .

 For irregular particles:
o Particles more than 75 mm: sieving
o Particles less than 75 mm: Laser diffraction
technique: e.g. Malvern Mastersizer, Coulter
Counter etc.

Different measurement techniques give different

sizes if the particles are non-spherical, which is
usually the case.

dsv and dv are generally considered to be the

most useful sizes where fluid/particle
interactions are involved. (eg. Flow thru fixed
and fluidized bed, pneumatic conveying etc.)
and they are related to each other thru the
particle sphericity, .

Malvern Master Sizer S: it measures dv if

sphericity is known, than dsv can be estimated.

Other way to find dsv is by using Ergun equation.

 According to Abrahamsen & Geldart (1980):

o For quartz: = 0.8

o dv = 1.13dp (2.5)

The average sphericity for regular figures:

d sv
0.773
dv (2.6)

Thus, for non-spherical particles,

dsv 0.87dp (2.7)

For spherical or near-spherical particles;

dv = dsv = dp (2.8)
Example 2.1

Calculate the equivalent volume sphere diameter dv

and the surface volume equivalent sphere, dsv of a
cuboid particle of side length 1,2 and 4 mm.
 For irregular particles:
o Particles more than 75 mm: sieving
o Particles less than 75 mm: Laser diffraction
technique: e.g. Malvern Mastersizer, Coulter
Counter etc.

Different measurement techniques give different

sizes if the particles are non-spherical, which is
usually the case.

dsv and dv are generally considered to be the

most useful sizes where fluid/particle
interactions are involved. (eg. Flow thru fixed
and fluidized bed, pneumatic conveying etc.)
and they are related to each other thru the
particle sphericity, .

Malvern Master Sizer S: it measures dv if

sphericity is known, than dsv can be estimated.

Other way to find dsv is by using Ergun equation.

 According to Abrahamsen & Geldart (1980):

o For quartz: = 0.8

o dv = 1.13dp (2.5)

The average sphericity for regular figures:

d sv
0.773
dv (2.6)

Thus, for non-spherical particles,

dsv 0.87dp (2.7)

For spherical or near-spherical particles;

dv = dsv = dp (2.8)
Example 2.1

Calculate the equivalent volume sphere diameter dv

and the surface volume equivalent sphere, dsv of a
cuboid particle of side length 1,2 and 4 mm.
2.3.2 Mean size and size distribution

No industrial powder is monosized and it is

usually necessary to characterize the powder by
both the size distribution and a mean size.

If a powder of mass M has a size range

consisting of Np1 of size d1, Np2 of size d2 and
so on, the mean surface/volume size is
expressed by:

Np1d13 Np 2 d 32 Np 3 d 33 ...
d sv (2.9)
Np1d12 Np 2 d 22 Np 3 d 32 ...

d sv
x
(2.10)
x d

where x is the weight fraction of particles in

each size range.
 When sieving is used, d1, d2, are replaced by
the arithmetic averages of adjacent sieve
apertures, dpi and the equation becomes:

1
dp (2.11)
xi d pi

and dp is mean particle size and not directly

related to the dsv.
Mean particle size, dp: emphasis to the
important influence which small proportions of
fines have.

Equation (2.11) should not be used if the

powder has an unusual distribution, for example
bi- or tri-modal or has an extremely wide size
range.
 This type of powder will not behave in a
homogeneous way and cannot be characterized
by a single number.

Refer to Table 1 for example.

The British Standard Sieve series is arranged in

multiples of 2 , and this is used as a basis in
Table 2.

This will give an idea of relative spread as

judged from the number of sieves. (Refer Table
2).

It is always advisable to first plot the size

distribution of powder as a weight fraction, or
percentage in a size range, against the average
size, i.e. x vs. dpi because a plot of cumulative
percentage undersize can conceal peculiarities
of distribution.
 Table 1: Size Distribution of sieved sand
Sieve Size dpi, Wt % in Cum. %
aperture, mm mm range, xi undersize

-600 + 500 550 0.50 100

-500 + 420 460 11.60 99.5
-420 + 350 385 11.25 87.9
-350 + 300 325 14.45 76.65
-300 + 250 275 20.80 62.2
-250 + 210 230 13.85 41.4
-210 + 180 195 12.50 27.55
-180 + 150 165 11.90 15.05
-150 + 125 137 3.15 3.15
Table 2: Width of Size Distributions Based on Relative
Spread
Number of sieves on Type of
which the middle 70% distribution
(approx.) of the d pm
powder is found
1 0 Very narrow
2 0.03 Narrow
3 0.17 Fairly narrow
4 0.25 Fairly wide

5 0.33
6 0.41 Wide
7 0.48
9
11
0.60
0.70
Very wide

> 13 > 0.80 Extremely wide

 Other method of characterizing powder, the
median, dpm: corresponds to the 50% value on
the graph of cumulative percentage undersize
versus size.

There is no universally agreed way of

comparing the width of the size distribution of
two powders having different mean sizes, nor of
defining how wide a distribution is.

In order to compare the width of the size

distribution of two powders having different
mean size or defining how wide a distribution is;

relative spread, d pm from cumulative
percentage undersize plot is used as suggested
by Geldart (2003).
 d 84% d16%
(2.12)
2

See Figure 2 for example.

In the example given, = 105 mm and /dpm =

0.39.
2.4 Particle Size Analysis

2.4.1 Equivalent of Means

A population of particles is described by a

particle size distribution.

Particle size distributions may be expressed as

frequency distribution curves, f(x) or dF/dx or
cumulative curves, F(x).

The distributions can be by number, surface,

mass or volume (if particle density does not
vary, then the mass distribution is the same as
the volume distribution).

In most practical applications, the population of

powders must be described by a single number.
 Some of the central tendency expression which
depending on the particular application are as
below:

o Mode: The most frequently occurring size in

the sample. The mode has no practical
significance as a measure of central
tendency and is rarely used in practice.

o Median: Easily read from the cumulative

distribution as the 50% size, which splits the
distribution into two equal parts. Also has
no special significance as a measure of
particle size.
 Many different means can be defined for a
given size distribution. All the means below
can be described by the equation;
1

gx dF
gx 0
1 (2.13)

0
dF

but 0
dF 1 (2.14)

g x g x dF
1
and thus, 0 (2.15)

where x is the mean and g is the weighting

function, which is different for each mean
definition (refer Table 3)
 Table 3: Definition of means
g(x) Mean and notation
dp Arithmetic mean, dp,a
2
dp Quadratic mean, dp,q
3
dp Cubic mean, dp,c
Log dp Geometric mean, dp,g
1/ dp Harmonic mean, dp,h

Equation (2.15) tells us that the mean is the

area between the curve and the cumulative
distribution, F(x) axis in a plot of F(x) versus the
weighting function g(x) (refer Figure 3).
 Equation (2.15) tells us that the mean is the
area between the curve and the cumulative
distribution, F(x) axis in a plot of F(x) versus the
weighting function g(x) (refer Figure 3).

Figure 3: Plot of cumulative frequency vs. weighting

function, g(x).
 Each mean conserve two properties of original
population of particles.

Example 1: arithmetic mean of surface

distribution conserves the surface and volume
of original population (see example 3.3). This
mean is also known as surface-volume mean or
Sauter mean.

Example 2: quadratic mean of number

distribution conserves the number and surface
or original population and is known as number-
surface mean.
 A comparison of the values of the different
means and the mode and median for a given
particle size distribution is shown by Figure 4.

The Figure shows that:

o The values of the different expression of

central tendency can vary significantly.

o Two quite different distributions could have

the same arithmetic means, median etc.

o Thus, the most appropriate mean particle

size must be selected for appropriate
process or application.
Figure 4: Comparison between measures of
central tendency.
 Physical properties of particulate

Shape
Size
Density
Porosity
Hardness
Sphericity
Roughness
 Porosity

Porosity is the ratio of pore

volume to its total volume.
Porosity is controlled by:
rock type, grain size, pore
distribution, cementation,
diagenetic history and
composition.
Measurement: BET, mercury
porosimeter
 Hardness

is a measure of how
resistant solid matter is to
various kinds of permanent
shape change when a force is
applied.
Macroscopic hardness -
strong intermolecular bonds
different measurements of
hardness: scratch
hardness, indentation hardness,
and rebound hardness
 Sphericity
is a measure of how spherical (round) an object
is.
Wadell in 1935, the sphericity of a particle is: the
ratio of the surface area of a sphere (with the
same volume as the given particle) to the surface
area of the particle:
Measurement: image analysis
 Roughness
Physical/Morphology of the
surface of particulates
Determine the contact force
(interparticle forces)
Explain/Show the particle
interaction with other particles
or any environment
 How to measure?
(Atomic Force Microscopy)
 Particles Crystallinity

Crystal vs. Amorphous

 How to measure?
(X-Ray Diffraction XRD)
Measure the average
spacings between layers or
rows of atoms
Determine the orientation
of a single crystal or grain
Find the crystal structure
of an unknown material
Measure the size, shape
and internal stress of
small crystalline regions