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Chapter 1 1.

Introduction Outline
Characterization Of Individual Particles The design of any operation involving 1 Introduction
particles requires precise information on 2 Particle density
their properties
3 Particle size
The most important properties are density, 4 Particle shape
size and shape
5 Adhesion of particles
Cedric Briens September 7, 2016
This chapter defines these properties and 6 Dustiness
reviews the techniques for their
measurement
1 2 3

What is the
2. Particle density What is the Skeletal density? apparent particle density?
Density of the material from which particles mass of particle
Up
Skeletal density are formed: Usk volume of particle (including pores)
non-porouss non-porouss

Apparent particle density

non-porouss non-porouss
Bulk density

4 5 6

Relationship between Up and Usk What is the bulk density? Relationship between Ub and Up

mass of solid mass of solid volume of bed  volume of voids


1 1 volume of bed volume of particles volume of bed
 Zp Density of the bulk
Up Usk powder:
includes the voids in- Ub Up 1  H
volume of solid material  volume of pores between the particles
solid mass
H: voidage or volume fraction of bulk powder
volume of solid material volume of pores occupied by voids.

solid mass solid mass
7 8 9
Example: Bulk density measurement Bulk density measurement
fluidized cracking catalyst
The bulk density depends on how the powder
Usk = 2500 kg/m3 is packed
Zp = 0.50x10-3 m3/kg
Up = 1100 kg/m3 Two extremes:
Ub = 500 kg/m3 Loose or aerated bulk density
Compact or tapped bulk density

10 11 12

Loose or aerated bulk density Compact or tapped bulk density Skeletal density measurement

movie

Two pycnometry measurement techniques


may be used:

1) liquid pycnometry: inaccurate

2) gas pycnometry: elaborate but accurate


movie
13 14 15

Liquid pycnometry Liquid pycnometry Liquid pycnometry

weighing o mass of added water o volume of added water

volume of flask volume of added water  volume of solids material

16 17 18
Liquid pycnometry Gas pycnometry
Particle density measurement

Porous particles: 1) Mercury pycnometry: assume that


mercury does not penetrate into the pores
The liquid may (Mercury is sometimes replaced by
not fill all the silicone oil). Inaccurate
pores 2) Caking detection: caking occurs when
the pores are filled with liquid. Inaccurate
3) Gas adsorption isotherms
19 20 21

Outline
1 Introduction
FCC
2 Particle density
tertiary
3 Particle size FCC
4 Particle shape
cyclone
5 Adhesion of particles catch
6 Dustiness

22 23 24

Talcum
Polymer C Polymer W
powder

25 26 27
Characterizing the size of a Particle size cuts
particle with a complex shape Size cut i contains 0.18

the particles with a 0.16

diameter between 0.14


Volume-equivalent particle diameter: diameter of
dpi - 'dpi /2 0.12
the sphere which has the same volume as the particle
0.10
and
Polymer E 0.08
dpi + 'dpi /2
Others: 0.06

Aerodynamic diameter: diameter of the sphere with a density of 0.04


1000 kg/m3 which falls at the same speed as the particle in ambient

fraction of particles in size cut (xi)


xi may be based on:
0.02
air weight
Sieve diameter volume 0.00
0 50 100 150 200 250 300 350 400 450 500 550 600
Diameters based on projected area area
number particle diameter (dp), Pm

28 29 30

Mean diameters Sauter-mean diameter and


specific area Median particle diameter
arithmetic mean : d pam x i d pi (note : x i 1)
i i mean specific surface (a):
geometric or log  mean : ln d plm x i ln d pi
i particle surface in 1 kg of mixed size solids Diameter such that 50% of particles are
For the arithmetic and log  mean diameters, x i may be any type of fraction
larger than this diameter and 50% are
For the Sauter  mean diameter, x i must be the volume fraction :
6 smaller
spherical particles: a
1 x Up d psm The median diameter depends on the type of
d psm
i d i
pi 6 fraction xi
non-spherical particles: a
Up I d psm

31 32 33

Comparison of various mean diameters for a typical size distribution Cumulative distribution Differential distribution
arithmetic mean diameter, Pm 221

100
from log-mean or geometric mean diameter, Pm 168
90
0.3
80
volume % harmonic or Sauter mean diameter, Pm 99
70

median diameter, Pm 192 60


0.2
50

40
arithmetic mean diameter, Pm 1.3
30
derivative, wt%/Pm

0.1
from log-mean or geometric mean diameter, Pm 1.0 20

10
weight % with a diameter smaller than dp

number % harmonic mean diameter, Pm 0.9 0


0 100 200 300 400 500 600 0.0
0 100 200 300 400 500 600
median diameter, Pm 0.8 particle diameter (dp), Pm
34 35 particle diameter (dp), Pm 36
Combining two particle size
Relationship between number and Theoretical size distribution
distributions of the same sample
weight distributions functions

Use Excel (or FBMODX) For example, two measurement techniques Useful for smoothing and interpolation
may provide the size distribution of a
sample for 2 different ranges of particle size Do not use for extrapolation

The easiest way is to use the cumulative


distribution

37 38 39

Normal or gaussian distribution Log-normal distribution Rosin-Rammler distribution

d 2
ln pi
pi pam
d  d 2
exp  2
d plm
2V exp  2
F(d p ) 1  exp  ad sp
dp 2 ln V
F(d p ) d(d ) g
pi
0 V 2S dp
d(d )
pi
F(d p ) 0 ln V g 2S
d pi

40 41 42

Normal paper Log-normal paper


Weibul distribution If the distribution is gaussian, the cumulative distribution If the distribution is log-normal, the cumulative distribution
will plot as a straight line will plot as a straight line.
99.9
99.9
log-normal probability paper
normal probability paper
99
99
d d
X p p min 90
d pm 90

70
70
50
50
30
30

10
10
Plotting with probably scale axis:
F d p 1  exp  X E
1) Use Sigmaplot or Origin commercial software 1
1

0.1
or 0.1
weight % with a diameter smaller than dp

2) Use provided Probability Scale charts.xls 0.01


weight % with a diameter smaller than dp

0.01
0.001
0.001
1 10 100
0 100 200 300 400 500 600
43 particle diameter (dp), Pm 44 particle diameter (dp), Pm 45
Particle size measurement Particle size measurement 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) (movie;
brazil nut movie; humans in snow avalanches)
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 movie).
With fine particles, sample dispersion is also movie
important. 46 47 48

Particle size measurement Sieving Sieving


Various methods:
1) Sieving: usually for dp > 50 Pm
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 49 50 51

Sieving Sieving Light scattering


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 The most popular technique
movie
Measures particle diameters from 0.5 to 3000 Pm
52 53 54
Both dry and wet measurements
Dry methods: screening, elutriation, Wet methods:
centrifugation in a gas, impaction, light sedimentation/centrifugation, electrical Outline
scattering conductivity, light scattering
1 Introduction
2 Particle density
Particle-particle agglomerates can be broken apart:
A frequent problem with these methods: surfactant additives + ultrasonic vibrations
3 Particle size
Particle-particle agglomeration: But: 4 Particle shape
Van der Waals forces
Surfactants may promote agglomeration 5 Adhesion of particles
Electrostatic forces
Ultrasonic vibrations may promote agglomeration or
Prevalent for small particles (high surface/volume) break particles
6 Dustiness
Additives can help
55 56 57

Particle shape: examples Shape factors from direct shape


4. Particle shape characterization
Introduction - inks, paints, cosmetics: flaky particles cover more Usually from image analysis
area
Various shape factors Example: for each particle, draw diameters
- abrasives: better if highly angular through its center of gravity, 30 degrees apart,
Shape factors from direct shape characterization - fibers for plastics reinforcement: elongated for and take the ratio of the smallest to the largest
Shape factors from particle-fluid interactions good impact strength.
of these diameters
Shape factors from product quality tests - rubber grains: must be round for good tensile
strength (otherwise, grains would align along one x Particle sphericity:
Measurement of particle shape direction and eventually tear) surface area of sphere with the same volume as the particle
)
- perfectly spherical particles have a smoother feel actual surface area of the particle
attractive for cosmetic applications
58 59 60

Shape factors from particle-fluid Shape factors from product


Outline
interactions quality tests
Flakiness index 1 Introduction
Many shape factors based on measured round particles: 2 Particle density
particle-fluid interactions 3 Particle size
See the chapter on Particulate-Fluid 4 Particle shape
"flaky" particles:
interactions 5 Adhesion of particles
6 Dustiness
Angularity index: based on Hausner ratio:
Angular particles are more cohesive
61 62 63
5. Adhesion of particles Outline 6. Dustiness
solids
1 Introduction sample
Adhesion of particles on other particles or on 2 Particle density
a flat surface may be very important for some 3 Particle size
processes 4 Particle shape
5 Adhesion of particles dust
There are very few techniques to characterize 6 Dustiness suction
such adhesion (e.g. the turntable) filter

64 65 66

Normal paper Log-normal paper

99.99 99.99
99.95 99.95
99.9 99.9
99.8 99.8

99 99
98 98
95 95
90 90
80 80
70 70
60 60
50 50
40 40

% below dp
30 30

% below dp
20 20
10 10
5 5
2 2
1 1
0.5 0.5
0.2 0.2
0.1 0.1
0.05 0.05
0.01 0.01
0 10 20 30 40 50 60 70 80 90 100 1 10 100
67 68
dp
dp

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