1

Chapter 1
Characterization Of Individual Particles




Cedric Briens April 16, 2010

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1. Introduction
1. The design of any operation involving
particles requires precise information on
their properties
2. The most important properties are density,
size and shape
3. This chapter defines these properties and
reviews the techniques for their
measurement

3
Outline
1 Introduction
2 Particle density
3 Particle size
4 Particle shape
5 Adhesion of particles
6 Dustiness
4
2. Particle density

Skeletal density

Apparent particle density

Bulk density
5
What is the Skeletal density?
Density of the material from which particles
are formed:
sk


non-porouss
non-porouss
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What is the
apparent particle density?
non-porouss
p
mass of particle
volume of particle (including pores)
=
non-porouss
7
Relationship between
p
and
sk

p
p sk
1 1
= + e

volume of solid material volume of pores
solid mass
+
=
volume of solid material volume of pores
solid mass solid mass
+
8
What is the bulk density?

Density of the bulk
powder:
includes the voids in-
between the particles
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Relationship between
b
=
p
( )
b p
1 = c
c: voidage or volume fraction of bulk powder
occupied by voids.
mass of solid mass of solid volume of bed volume of voids
volume of bed volume of particles volume of bed
| |
=
|
\ .
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Example:
fluidized cracking catalyst

sk
= 2500 kg/m
3

e
p
= 0.50x10
-3
m
3
/kg

p
= 1100 kg/m
3

b
= 500 kg/m
3

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Bulk density measurement
The bulk density depends on how the powder
is packed

Two extremes:
Loose or aerated bulk density
Compact or tapped bulk density
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Bulk density measurement
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Loose or aerated bulk density
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Compact or tapped bulk density
15
Skeletal density measurement

Two pycnometry measurement techniques
may be used:

1) liquid pycnometry: inaccurate

2) gas pycnometry: elaborate but accurate


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Liquid pycnometry
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Liquid pycnometry
weighing mass of added water volume of added water
volume of flask volume of added water volume of solids material

= +
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Liquid pycnometry
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Liquid pycnometry
Porous particles:

The liquid may
not fill all the
pores
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Gas pycnometry
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Particle density measurement

1) Mercury pycnometry: assume that
mercury does not penetrate into the pores
(Mercury is sometimes replaced by
silicone oil). Inaccurate
2) Caking detection: caking occurs when
the pores are filled with liquid. Inaccurate
3) Gas adsorption isotherms
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Outline
1 Introduction
2 Particle density
3 Particle size
4 Particle shape
5 Adhesion of particles
6 Dustiness
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FCC
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FCC
tertiary
cyclone
catch
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Talcum
powder
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Polymer C
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Polymer W
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Polymer E
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Characterizing the size of a
particle with a complex shape

Volume-equivalent particle diameter: diameter of
the sphere which has the same volume as the particle

Others:
Aerodynamic diameter: diameter of the sphere with a density of
1000 kg/m
3
which falls at the same speed as the particle in ambient
air
Sieve diameter
Diameters based on projected area

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Particle size cuts
Size cut i contains
the particles with a
diameter between
d
pi
- Ad
pi
/2
and
d
pi
+ Ad
pi
/2

particle diameter (d
p
), m
0 50 100 150 200 250 300 350 400 450 500 550 600
f
r
a
c
t
i
o
n

o
f

p
a
r
t
i
c
l
e
s

i
n

s
i
z
e

c
u
t

(
x
i
)
0.00
0.02
0.04
0.06
0.08
0.10
0.12
0.14
0.16
0.18
x
i
may be based on:
weight
volume
area
number
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Mean diameters
( ) ( )
pam i pi i
i i
plm i pi
i
i
i
i
psm pi
: d x d (note : x 1)
: ln d x ln d
For the arithmetic and log mean diameters, x may be any type of fracti
arithmetic mean
geometric or log mean
Sauter me
on
For the , x be the volume frac mu ti st on :
1 x
an
d d
diameter
= =
=
=

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Sauter-mean diameter and
specific area
p psm
p psm
mean specific surface (a):
particle surface in 1 kg of mixed size solids
6
spherical particles: a
d
6
non-spherical particles: a
d
=

=
|
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Median particle diameter

Diameter such that 50% of particles are
larger than this diameter and 50% are
smaller
The median diameter depends on the type of
fraction x
i
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Comparison of various mean diameters for a typical size distribution


arithmetic mean diameter, m

221

from

log-mean or geometric mean diameter, m

168

volume %

harmonic or Sauter mean diameter, m

99



median diameter, m

192



arithmetic mean diameter, m

1.3

from

log-mean or geometric mean diameter, m

1.0

number %

harmonic mean diameter, m

0.9



median diameter, m

0.8

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Cumulative distribution
particle diameter (d
p
), m
0 100 200 300 400 500 600
w
e
i
g
h
t

%

w
i
t
h

a

d
i
a
m
e
t
e
r

s
m
a
l
l
e
r

t
h
a
n

d
p
0
10
20
30
40
50
60
70
80
90
100
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Differential distribution
particle diameter (d
p
), m
0 100 200 300 400 500 600
d
e
r
i
v
a
t
i
v
e
,

w
t
%
/

m
0.0
0.1
0.2
0.3
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Relationship between number and
weight distributions
Use Excel (or FBMODX)
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Combining two particle size
distributions of the same sample


For example, two measurement techniques
may provide the size distribution of a
sample for 2 different ranges of particle size

The easiest way is to use the cumulative
distribution
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Theoretical size distribution
functions

Useful for smoothing and interpolation

Do not use for extrapolation
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Normal or gaussian distribution
( )
p
2
pi pam
2
d
p pi
0
d d
exp
2
F(d ) d(d )
2
| |

o
|
\ .
=
o t
}
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Log-normal distribution
( )
( )
( )
( )
F d
d
d
d d
d
p
pi
plm
g
g
pi
pi
d
p
( )
exp
ln
ln
ln
( )
=

|
\

|
.
|
|
|
\

|
.
|
|
|
\

|
.
|
|
|
|
|
|
}
2
2
0
2
2
o
o t
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Rosin-Rammler distribution
( )
s
p p
d a exp 1 ) d ( F =
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Weibul distribution
pm
min p p
d
d d
X

=
( ) ( )
|
= X exp 1 d F
p
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Normal paper
If the distribution is gaussian, the cumulative distribution
will plot as a straight line
particle diameter (d
p
), m
0 100 200 300 400 500 600
w
e
i
g
h
t

%

w
i
t
h

a

d
i
a
m
e
t
e
r

s
m
a
l
l
e
r

t
h
a
n

d
p
0.001
0.01
0.1
1
10
30
50
70
90
99
99.9
normal probability paper
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Log-normal paper
If the distribution is log-normal, the cumulative distribution
will plot as a straight line.
particle diameter (d
p
), m
1 10 100
w
e
i
g
h
t

%

w
i
t
h

a

d
i
a
m
e
t
e
r

s
m
a
l
l
e
r

t
h
a
n

d
p
0.001
0.01
0.1
1
10
30
50
70
90
99
99.9
log-normal probability paper
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Particle size measurement
Accurate sampling is a crucial operation: more
errors can be attributed to sampling than to the
actual size analysis.
The two "golden rules of sampling" (Allen):
1) "a powder should be sampled while in motion" (to
prevent segregation in non- moving powders)
2) "the whole of the stream should be taken for many
short increments of time in preference to part of the
stream being taken for the whole of the time"
(segregation).
With fine particles, sample dispersion is also
important.

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Particle size measurement
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Particle size measurement
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Particle size measurement
Various methods:
1) Sieving: usually for d
p
> 50 m
2) Sedimentation or centrifugation in a liquid
3) Centrifugation in a gas
4) Elutriation
5) Impaction
6) Electrical conductivity
7) Light scattering and blockage
8) Image analysis

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Sieving
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Sieving
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Sieving
time consuming
shaking duration must be long enough to prevent
large errors
cannot be used with solids which attrit or
agglomerate easily
if angular particles, does not give volume-
equivalent diameter
Sieving results are often reported in terms of mesh
numbers: a large mesh number means a small
particle size

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Light scattering
The most popular technique
Measures the projected area of the particles and
thus provides the volume-equivalent diameter
when the measurement cell is designed so as to
present the particles in a random orientation
Measures particle diameters from 0.5 to 3000 m
Both dry and wet measurements
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Dry methods: screening, elutriation,
centrifugation in a gas, impaction, light
scattering


A frequent problem with these methods:
Particle-particle agglomeration due to Van der
Waals or electrostatic forces
Prevalent for small particles (high surface/volume)
Additives can help
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Wet methods:
sedimentation/centrifugation, electrical
conductivity, light scattering


Particle-particle agglomerates can be broken apart
by a combination of surfactant additives and
ultrasonic vibrations
Surfactants may also promote agglomeration
Ultrasonic vibrations may promote agglomeration
or break particles
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Outline
1 Introduction
2 Particle density
3 Particle size
4 Particle shape
5 Adhesion of particles
6 Dustiness
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4. Particle shape
Introduction
Various shape factors
Shape factors from direct shape characterization
Shape factors from particle-fluid interactions
Shape factors from product quality tests
Measurement of particle shape
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Particle shape: examples
- inks, paints, cosmetics: flaky particles cover more
area
- abrasives: better if highly angular
- fibers for plastics reinforcement: elongated for
good impact strength.
- rubber grains: must be round for good tensile
strength (otherwise, grains would align along one
direction and eventually tear)
- perfectly spherical particles have a smoother feel
attractive for cosmetic applications

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Shape factors from direct shape
characterization
Usually from image analysis
Example: for each particle, draw diameters
through its center of gravity, 30 degrees apart,
and take the ratio of the smallest to the largest
of these diameters

surface area of sphere with the same volume as the particle
actual surface area of the particle
Particle sphericity:
u =
-
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Shape factors from particle-fluid
interactions

Many shape factors based on measured
particle-fluid interactions
See the chapter on Particulate-Fluid
interactions
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Shape factors from product
quality tests
Flakiness index
round particles:
"flaky" particles:
Angularity index: based on Hausner ratio:
Angular particles are more cohesive
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Outline
1 Introduction
2 Particle density
3 Particle size
4 Particle shape
5 Adhesion of particles
6 Dustiness
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5. Adhesion of particles

Adhesion of particles on other particles or
on a flat surface may be very important for
some processes
There are very few techniques to
characterize such adhesion (e.g. the
turntable)
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Outline
1 Introduction
2 Particle density
3 Particle size
4 Particle shape
5 Adhesion of particles
6 Dustiness
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6. Dustiness
f i l t e r
s o l i d s
s a m p l e
s u c t i o n
d u s t