CHAPTER 2

PARTICLE SIZE CHARACTERIZATION

2.1 INTRODUCTION TO PARTICLE SIZE AND SHAPE

1. In many powder handling and
processing operations, particle size
and size distribution play a key role in
determining the bulk properties of the
powder.
2. Example of regular-shaped particles.

Source: http://blog.skylighter.com/fireworks/2007/11/how-particle-size-shape-is-defined.html

3. 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.

4. methods of measurement

LASER
DIFFRACTION

ELECTROZONE
SENSING

MICROSCOPY

EQUIPMENT

SEDIMENTATION

SIEVE

1. Laser Diffraction
Refer textbook section 1.8.6 (pg 16)
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 distribution

Malvern Mastersizer S
(Malvern Instrument Inc.)

2. Electrozone sensing
Refer text book section 1.8.5
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

3. Sieve
Refer text book section 1.8.1
Dry sieving using woven wire
sieves is a simple and cheap
method for particles size greater
than 45mm.
It gives mass distribution and a size
known as sieve diameter
Sieve diameter 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

4. Sedimentation
Refer text book section 1.8.3
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 apply (Re<0.3)
Method using water is suitable for
particles less than 50 mm

5. Microscopy
Optical microscopy can be used to measure
particle sizes down to 5mm.
Coupled with image analysis, the optical
microscope or electron 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

1. 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.
2. Powders are unlike fluid where the properties change easily
under applied load.
3. They may consolidate with time, and attrition and
segregation may occur in transfer.
4. Sampling is an important element of powder handling such
that it demands careful scientific design and operation of
the sampling system.

5. 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.
6. 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.
7. This means that all particles in the total must have
the same probability of being included in the final
sample.

8. To satisfy the above requirements, the

following basicgolden rules of sampling
should be followed wherever practicable.

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.
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.

9. 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;

 Some common diameters used in microscopy analysis are:

Equivalent circle diameter

Martins diameter
Ferret diameter
Shear diameter

, 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;
1. 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.
2. Split this down using a riffler to obtain a few hundreds
particles.
3. Count the exact number (n) and weight them (M).
Knowing the particle density, p, calculate the
equivalent sphere volume diameter, dv from

4. 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.
5. The Carman-Kozeny equation relates pressure
drop to particle size, dsv, voidage, and bed
depth, L at low Reynolds number.
6. Thus, dsv can be calculated from pressure drop
data.
7. From equation above, calculate .

P 1501 U

L
3
d sv2
2

(2.4)

 For irregular particles:

Particles more than 75 m: sieving method

Particles less than 75 m: 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):

For quartz: = 0.8
dv = 1.13dp
(2.5)
The average sphericity for regular figures:

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.

Example 2.2
Particle (density=2000kg/m3) with sphericity of 0.9
are poured into a container. A sample of 2000
particles taken from the powder weighed 1000 mg.
Determine volume diameter and surface/volume
diameter

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:

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:

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 21/4 ,
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 aperture,
m

Size dpi, m

Wt % in range,
xi

Cum. %
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
which the middle 70%
(approx.) of the powder
is found

d pm

1
2
3
4
5
6
7
9
11

0
0.03
0.17
0.25
0.33
0.41
0.48
0.60
0.70

> 13

> 0.80

Type of distribution

Very narrow
Narrow
Fairly narrow
Fairly wide
Wide

Very wide

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,

from cumulative percentage
d pm
undersize plot is used as suggested by Geldart (2003).

d84% d16%

2
In the example given,
= 105 m and /dpm = 0.39

Figure 2: Size distribution of a sand characterized in various ways

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:
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.
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;

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

dp 2

Quadratic mean, dp,q

dp 3

Cubic mean, dp,c

Log dp

Geometric mean, dp,g

1/ dp

Harmonic mean, dp,h

F(x)

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, F(x) 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:
The values of the different expression of central
tendency can vary significantly.
Two quite different distributions could have the
same arithmetic means, median etc
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

1.
2.
3.
4.
5.
6.
7.

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

(Atomic Force Microscopy)

Particles Crystallinity
Crystal

vs.

Amorphous

Definition of crystal
Solid with short and long range order with
atoms of molecules in a fixed lattice
arrangement
The distinction between a crystal and
amorphous solid is that between order and
disorder over large distances
Internal structure of crystals accessible by xray diffraction analysis.

(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