PT316 - Topic 2 - Particle Characterisation - Revised PDF

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PARTICLE CHARACTERISATION
Dept of Process Engineering

Stellenbosch University
Particle Technology 316
Particle Characterization: The Challenge

Liquids are completely specified by stating the composition, e.g. 98 %
ethanol in water
With particles and solids, composition is insufficient to specify the
particles/solids
e.g. Calcium carbonate
LDPE

Particle Characterization: The Challenge

Problem: how do we specify the size of a powder ?

Particle Characterization: Overview

Design and operation of industrial processes often require
single number summary of particle populations
Particle populations are rarely uniform in shape and size

Describing size of one particle is challenging
Describing sizes of particle populations is challenging
Statistical distribution functions allow description of
populations
Different methods for measuring particle population sizes

Different methods of measuring particle surface areas

Particle Characterization: Scope

Sphericity
Single particle size description
Particle population size description
Cumulative and differential frequency distributions

Converting between size distributions
Single number summary of distributions
Equivalence of means
Displaying size distributions
Particle size measurement

Particle surface area measurement
Sampling

Particle Characterization: Sphericity

Difficult to describe particle shapes
Difficult to summarize shapes in one number
One option - Sphericity
Ratio of (surface area of a sphere of volume equal to that of particle) to
(surface area of particle)
=
1
3
2
3
= sphericity
As = surface area of equivalent
volume sphere
Ap = surface area of particle
Vs = volume of sphere
Vp = volume of particle
Sphere volume to sphere area

(= ) =
=
3
6
6 3
1
3
= 6
Example: sphericity of cube is 0.806

2
3
Particle Characterization: Single Particle Description
Regular-shaped particle
Can describe size exactly using one or more dimensions

Particle Characterization: Single Particle Description
Irregular-shaped particle
Size description difficult; no single dimension adequate
Description dependent on measurement technique and
purpose
Microscopy
Sieving
Images from Wikipedia

(freely licensed media)
Sedimentation
balance
Coulter
counter
Permeametry
Particle Characterization: Single particle
General approach: what diameter of sphere would have

equivalent specific properties to that of the particle ?
Equivalent sphere diameters
Sphere passing through same sieve aperture (xP)

Equivalent sphere surface diameter (xS)
Equivalent sphere volume diameter (xV)
Equivalent sphere surface-volume diameter (xSV)
Same surface to volume ratio
Figure from
Rhodes (2008)


Size descriptions from microscopy
Function of projected surface
Figures from
Rhodes (2008)


Size descriptions from sieving
Equivalent sphere diameter
Sphere passing the same sieve aperture
Size descriptions from sedimentation

Equivalent sphere settling velocity diameter
Size descriptions from Coulter counter

Equivalent sphere volume diameter
Size descriptions from permeametry

Equivalent sphere surface-volume diameter

Particle Characterization: Summary this far
For irregular particles, we can define the particle size

in terms of an equivalent sphere that has the same
properties as the particle:
xP = diameter of sphere passing through same aperture as the particle
xS = diameter of a sphere having the same surface area as the particle
xV = diameter of a sphere having the same volume as the particle
xSV = diameter of a sphere having the same surface area to volume ratio as the
particle

Particle Characterization: Summary this far

surface area of a sphere = 2
volume of a sphere = 3
e.g. (i) cuboid 1 x 3 x 5
(ii) cylinder 1 x 3

Particle Characterization: Particle size distributions
In reality, there will be a range of particle sizes for a

given powder, e.g. for a particular powder:
particle
size
(microns)
number of
particles
0-10
10-20
20-30
30-40
40-50
50-60
60-70
70-80
80-90
90100
100110
110120
120130
10
20
30
45
90
170
190
180
120
60
20
How do we summarise this data graphically ?

Particle Characterization: Particle size distributions

Differential frequency distribution, f(x)
Related to the relative quantity of particles in a population within a
specific size range
Derivative of cumulative frequency distribution F(x)
f(x) = dF/dx
f(x)
Figure from
Rhodes (2008)

Particle Characterization: Multiple Particles - Distributions

Cumulative frequency distribution, F(x)
F(x) = probability that any particle in the population will have a size
smaller than or equal to x
Integral of differential frequency distribution f(x)
=
0
Figure from
Rhodes (2008)
E.g. 50% chance that any particle in the distribution above will have a size smaller than or equal to 45 m
E.g. 80% chance that any particle in the distribution above will have a size smaller than or equal to 55 m
Particle Characterization: Multiple Particles - Distributions

0-10
10-20
20-30
30-40
40-50
50-60
60-70
70-80
80-90
90-100
100-110
110-120
120-130
130-140
number of particles
10
20
30
45
90
170
190
180
120
60
20
mean size in range
15
25
35
45
55
65
75
85
95
105
115
125
135
fraction in range
0.000
0.005
0.011
0.021
0.032
0.048
0.096
0.181
0.202
0.191
0.128
0.064
0.021
0.000
cumulative fraction
0.000
0.005
0.016
0.037
0.069
0.117
0.213
0.394
0.596
0.787
0.915
0.979
1.000
1.000
size range
1.200
0.200
1.000
0.150
0.800
F(x)
f(x)
0.250
940
0.100
0.600
0.400
0.050
0.200
0.000
0.000
0
50
100
particle size (microns)

150
50
100
150
particle size (microns)
Particle Characterization: Multiple particles - Distributions

Various particle size distributions, depending on the
quantity being measured:
Number: fN(x) [differential] and FN(x) [cumulative]

Surface: fS(x) [differential] and FS(x) [cumulative]
Mass: fM(x) [differential] and FM(x) [cumulative]
Volume: fV(x) [differential] and FV(x) [cumulative]
f(x)
Figure from
Rhodes (2008)

Particle Characterization: Particle distributions

Can get vastly different distributions for same particle
population
But: fM(x) = fV(x) when particle density same for all particle sizes
Figure from
Rhodes (2008)
Particle Characterization: Particle distributions
Can convert between distributions, e.g. from number

distribution:
To surface: N S
Assume particle shape constant across particle sizes

= 2 ;
S = factor relating linear dimension of particle to its surface area

S = total surface area of particle population
To volume: N V
Assume particle shape constant across particle sizes

= 3 ;
V = factor relating linear dimension of particle to its volume

V = total volume of particle population
To mass: N M
Assume particle density constant across particle sizes

= 3 ;
Finding kS, kV, kM
0 = 1

Particle Characterization: Particle distributions discrete intervals
For discrete size intervals (for spherical particles)

From number fraction n(xi) to mass fraction m(xi)
=
3
3
From surface fraction s(xi) to mass fraction m(xi)

From mass fraction m(xi) to number fraction n(xi)

=
/3
/3
Above, xi is arithmetic mean of size range

Particle Characterization: Single number summary
Particle population can be described by distribution

e.g. cumulative frequency distribution F(x)
Figure from
Rhodes (2008)
Single number summary of distribution

Required by certain engineering calculations
Normally derived from a measure of central tendency
e.g. mean and median
Modelling real population of different sizes by artificial
population of single size

Measures of central tendency

Mode = most frequently occurring size in population
Median = size such that cumulative frequency is 0.5
Half the particles in the population have sizes smaller than this
value, the other half of the particles have sizes larger than this value
Mean = different central tendency values, all described by:

( ) =
0
1
= 0
= mean; () = weighting function

Mean definitions
=
0
1
0
= 0
Arithmetic mean
1
= ; =
0
Quadratic mean
2
= ;
Cubic mean
= ;
= 2
0
= 3
0
Geometric mean
= log ; log = log
Harmonic mean
1
1
1
1
= ;
=

Means can be defined for any cumulative distribution: e.g.

Arithmetic mean of the number distribution
1
=
0
Arithmetic mean of the surface distribution mean

1
=
0
Cubic mean of the volume distribution

3
etc.
= 3
0
The appropriate mean to choose will depend on the

properties of the original population that need to be
conserved
Conservation of properties
Mean conserves two properties of population
Nature of properties depends on type of mean and
distribution:
[ ] Arithmetic mean of surface distribution FS(x)

Conserves surface and volume of original population
Surface-volume mean
[ ] Arithmetic mean of number distribution FN(x)

Conserves number and length of original population
Number-length mean
[ ] Quadratic mean of number distribution FN(x)

Conserves number and surface of original population
Number-surface mean
Means can be equivalent e.g.
= arithmetic mean of a surface distribution

= harmonic mean of a volume distribution
= surface volume mean
= =
[see Rhodes Section 1.6 for proof]

Different mean definitions give different values

Different distributions may have same means
Figure from
Rhodes (2008)

Particle Characterization: Displaying size distributions
Typical particle size distributions

Normal (Gaussian) distribution
=
1
exp
2
Figures from
Rhodes (2008)
50 2
22
= standard deviation
Particle sizes with equal differences

from mean occur with equal frequency
Log-normal distribution
=
1
exp
2
50 2
22
z = log(x)
z = standard deviation of z
More common in naturally occurring

particle populations
Particle Characterization: Displaying size distributions
Typical particle size distributions

Rosin-Rammler-Bennet cumulative distribution
= 1 exp

63
Gaudin-Schuhmann cumulative distribution

=
100
Broadbent-Callcott cumulative distribution

= 1 exp
100
Gaudin-Meloy cumulative distribution

= 1 1
100

Particle Characterization: Particle size measurement

SELF-STUDY Examinable !!!
Sieving
Microscopy
Sedimentation methods
Permeametry
Electrozone sensing
Laser diffraction
For each method:

Principle of measurement
Apparatus and Operation
Size ranges that it is suitable for
Limitations
(dont have to do detailed processing of data)
Particle Characterization: Particle surface area measurement
Importance of particle surface area characteristics

Heterogeneous catalysis
Gas or fluid reactants catalysed by solid catalyst
Higher catalyst surface area = higher catalyst efficiency
E.g. Contact process (sulfuric acid synthesis), Haber-Bosch process
(ammonia synthesis)
Activated carbon
Very porous, high surface to volume ratio
1 gram of activated carbon ~ 500 to 3000 m2 surface area
Used in:
Water purification
Air filters
Gold purification

Particle Characterization: Particle area measurement

SELF-STUDY Examinable !!!
BET :
Principle of measurement
Apparatus and Operation
Limitations
(dont have to do detailed processing of data)

Particle Characterization: Particle sampling
Particle size analysis performed on small sample of large

mass of powder
E.g. 2 g sample of 1 ton powder
Sample needs to be representative of bulk powder
Challenge:
Most powder transport and mixing processes cause segregation
based on size, density and shape
Golden rules of sampling

Powder must be in motion when sampled
Sample of whole moving stream should be taken
For short time increment

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Dept of Process Engineering

Particle Technology 316

Particle Characterization: The Challenge

With particles and solids, composition is insufficient to specify the

e.g. Calcium carbonate

Dept of Process Engineering

Particle Technology 316

Particle Characterization: The Challenge

Dept of Process Engineering

Particle Technology 316

Particle Characterization: Overview

single number summary of particle populations

Particle populations are rarely uniform in shape and size

Different methods for measuring particle population sizes

Dept of Process Engineering

Particle Technology 316

Particle Characterization: Scope

Cumulative and differential frequency distributions

Particle size measurement

Dept of Process Engineering

Particle Technology 316

Particle Characterization: Sphericity

Sphere volume to sphere area

Example: sphericity of cube is 0.806

Dept of Process Engineering

Particle Technology 316

Particle Characterization: Single Particle Description

Dept of Process Engineering

Particle Technology 316

Particle Characterization: Single Particle Description

Images from Wikipedia

Particle Technology 316

Particle Characterization: Single particle

General approach: what diameter of sphere would have

Sphere passing through same sieve aperture (xP)

Dept of Process Engineering

Particle Technology 316

Particle Characterization: Single particle

Dept of Process Engineering

Particle Technology 316

Particle Characterization: Single particle

Size descriptions from sedimentation

Size descriptions from Coulter counter

Size descriptions from permeametry

Dept of Process Engineering

Particle Technology 316

Particle Characterization: Summary this far

For irregular particles, we can define the particle size

xP = diameter of sphere passing through same aperture as the particle

xS = diameter of a sphere having the same surface area as the particle

xV = diameter of a sphere having the same volume as the particle

Dept of Process Engineering

Particle Technology 316

Particle Characterization: Summary this far

Dept of Process Engineering

Particle Technology 316

Particle Characterization: Particle size distributions

In reality, there will be a range of particle sizes for a

How do we summarise this data graphically ?

Dept of Process Engineering

Particle Technology 316

Particle Characterization: Particle size distributions