Particle Science and

Technology Laboratory
POWDER CHARACTERIZATION
Prof. B. Pitchumani
Particle Science and Technology Laboratory
Department of Chemical Engineering
Indian Institute of Technology, Delhi, INDIA
Particle Science and
Technology Laboratory
Bio-Data of Prof. B. Pitchumani
SubjectInstituteYearFine grinding in Jet MillPh.D. IIT Madras1974Cyclone SeparatorInstitut fur Mechanische Verfahren Technik,
Karlsruhe1980Size and shape analysis of powderParticle Analysis Center,West Virginia UniversityMay-July1983 &June 1985High
temperature cycloneFlowabilty of powdersChemical Engineering DepartmentTechnical University, DelftThe
Netherlands1990Development of filter for Automobile exhstChemical Engineering Dept.Technical University Erlangen, Nurenberg
Germany2000
Bio-Data
Subject Institute Year
Fine grinding in Jet
Mill
Ph.D. IIT Madras 1974
Cyclone Separator Institut fur Mechanische
Verfahren Technik, Karlsruhe
1980
Size and shape
analysis of powder
Particle Analysis Center,
West Virginia University
May-July
1983 &
June 1985

Flowabilty of powders
And high temperature
cyclone
Chemical Engineering
Department
Technical University, Delft
The Netherlands
1990
Development of filter Chemical Engg Dept.
Technical University
Erlangen, Nurenberg
Germany
2000
Particle Science and
Technology Laboratory
INTERACTIONS
GermanyUniversity of KarlsruheBerlin UniversityUniversity of
StuttgartUniversity of KonstanzUniversity of AachenUniversity of
ErlangenUniversity of Braunsweig
United KingdomUniversity of Kent, CanterburyUniversity of
SwanseaUniversity of LoughboroughThames Polytechnic
United States of AmericaWest Virginia University, Morgentown
University of Illinois, Chicago University of Pittsburgh, University of
Utah .University of Iowa, Iowa city University of Florida,
Gainesville, University of Houston
Switzerland ETH, Zurich
The Netherlands Technical University, Delft Technical University ,
Eindoven
Japan Univ. of Tokyo, Doshisa Univ,. Nagoya university Hakoida
university
Particle Science and
Technology Laboratory
PARTICLE
Solid Powder, granules, pellets

Liquid Droplet, Suspension

Gas-Bubble, Foam, Emulsion
Particle Science and
Technology Laboratory
Powder Characterization
Size, Size distribution

Shape (Morphology)

Surface area

Bulk density

Flowability

Zeta potential
Particle Science and
Technology Laboratory
DEFINITION OF PARTICLE SIZE


Diameter

Definition

Feret's diameter d
H
The mean value of the distance between pairs of
parallel tangents ;to the projected outline of the
particle.
Martin's diameter d
M


The mean chord length of the projected outline of the
particle.

Projected area diameter,
d
pr




Diameter of a circle having the same area as the
projected area of the particle (1) resting in a stable
position (2) in random orientation.
Sieve diameter, d
Sie


The width of the minimum square aperture through
which the particle will pass.

Stokes diameter, d
stk



The falling diameter of a particle in the laminar flow
region.

Surface diameter, d
S



Diameter of a sphere having same surface as the
surface of particle.

Volume diameter, d
V


Diameter of a sphere having the same volume as the
particle.

Aerodynamic diameter,
d
ae


Diameter of an unit density sphere with the same
settling velocity as the particle in question.



Particle Science and
Technology Laboratory
Significance of Size Distribution
0
20
40
60
80
100
120
0 5 10 15 20 25 30 35
Particle Size [microns]
C
u
m
u
l
a
t
i
v
e

U
n
d
e
r
s
i
z
e

[
w
t

%
]
Sample-1
Sample-2
Sample-3
Particle Science and
Technology Laboratory
Sample

Bulk Density

Dustiness

Dispersion

1

Lowest

maximum

lowest

2

Moderate tolerable

Fair
3

Highest

Minimum

Very good

0
20
40
60
80
100
120
0 5 10 15 20 25 30 35
Particle Size [microns]
C
u
m
u
l
a
t
i
v
e

U
n
d
e
r
s
i
z
e

[
w
t

%
]
Sample-1
Sample-2
Sample-3
Significance of Size Distribution
Particle Science and
Technology Laboratory
DISTRIBUTION EQUATIONS
The distribution function can be represented
either as a probability density function, q
r
(x)
or
as a cumulative distribution function Q
r
(x),
both of which are the functions of the particle
size `x'.
Particle Science and
Technology Laboratory
RELATIONSHIP IN
DISTRIBUTION EQUATIONS
q (x) =
dQ (x)
dx
r
r
Particle Science and
Technology Laboratory
DISTRIBUTION EQUATIONS
TABLE : Definition of r
S.N
o.
Experimental
method
Type of
measurement
r
1 Microscopy counting 0
2 Photo-
sedimentation
area 2
3 Sieving and
sedimentation
weight 3
Particle Science and
Technology Laboratory
Normal distribution
( )
(

2
2
50
0
2
x - x -
exp
2
1
= (x) q
o
t o
Particle Science and
Technology Laboratory
Log-Normal distribution
Q (x) =
1
2
exp
ln
ln
r
g
x
x
g
2
50
o t
o

(
(
(
x
50
, is the median particle size corresponding
to Q(x) = 50%.
o
g
84
50
=
x
x
|
\

|
.
|
Particle Science and
Technology Laboratory
( )
n
d
X
X
X Q
|
|
.
|

\
|
= exp
3
Rosin Rammler Equation
DISTRIBUTION EQUATIONS
Gaudin - Schumann Equation
( )
m
X
X
x Q
|
|
.
|

\
|
=
max
3
Nikiyama- Tanasawa Equation
( ) ( )
3
2
2
1 0
exp
K
X K X K x q =
Particle Science and
Technology Laboratory
Different type of Size Distribution
0
20
40
60
80
100
0 20 40 60 80 100 120 140 160
Particle Size, [m]
C
u
m
u
l
a
t
i
v
e

u
n
d
e
r
s
i
z
e
,

Q
3
(
x
)
,

[
%
]
Volume Distribution
Number Distribution
Length Distribution
Area Distribution
Particle Science and
Technology Laboratory
Different type of Size Distribution
Particle Science and
Technology Laboratory
To calculate distribution q
t
(x) from
given distribution q
u
(x).
q (x) =
x q (x)
x q (x) dx
t
t - u
u
t - u
u
x
x
min
max
INTER CONVERSION OF DISTRIBUTION
Particle Science and
Technology Laboratory
Shape characterization

Feret Diameter

Sieve Cascadograph

Fractals

Particle Science and
Technology Laboratory
INSTRUMENTS FOR
SIZE AND SIZE DISTRIBUTION
SHAPE ANALYSIS
ANGLE OF REPOSE
BULK AND TRUE DENSTY
FLOWABILITY
AIR PERMEALITY
ZETA POTNTIOAL
DUSTINESS
Particle Science and
Technology Laboratory
SURFACE AREA METER
Particle Science and
Technology Laboratory
SURFACEAREA METER
Particle Science and
Technology Laboratory
EQUATION

S = k
1
1 -

t
L
v2
2
2
3
2
2
2
1
2
c
c
|
\

|
.
|
|
\

|
.
|
A
where k is a constant given by
( ) ( )
k = S 1 -
L
t
v1 1 1
1
1
1
2
c c

|
\

|
.
|
3
2
A
Particle Science and
Technology Laboratory

Company Name: Aurobindo pharmaceutical Lit. 19.12.2005
Sample Name : Aurobino
PCI,Q3(x), [%]
0
1 2 2 4
2 3 5 9
3 5 10 20
4 7 15 32
5 9 30 56
6 11 52 71
7 13 91 82
8 15 138 88
9 16 240 96
10 18 363 100
15 27
20 35
25 42
30 48
35 54
40 59
45 64
63 77
75 83
90 89
106 93
125 95
150 98
212 100
250 100
Particle size, m
Q3(x), [%]
Malvern
New Sample 1
Particle Science and
Technology Laboratory
Geldart Classification of powders
Particle Science and
Technology Laboratory
TO IMPROVE THE FLOWABILITY
Larger number of fines cause increased adhesive-cohesive forces in the
powder leading to cohesive flow behavior
Particle Science and
Technology Laboratory
UNIT OPERATIONS
Crystallization (size and shape control)
Liquid solid separation (filtration/ centrifuging)
Drying (batch or continuous)
Pulverizing (shape and size distribution control)
Coating (nano particle coating)
Particle Science and
Technology Laboratory
There is variation in size distribution
Potency is high but purity is less
Morphology of particles produced during crystallization is changed after
final product is produced
Filtration time is much higher than theoretical time
Powder when transported for longer time becomes cake and volume of
packed material is reduced
Drying time is much higher than theoretical time

OBSERVATIONS
Particle Science and
Technology Laboratory
The life of filter cloth in centrifuge got reduced
The material has to be reground for desired size
Retrofitting of storage silo to prevent choking
Reduce the pressure drop in cyclones and bag house
Estimation of hammer size and shape
Interpretation of size distribution for energy saving
Simple method to estimate size distribution in subsieve
size range
Selection of fabric for bag house
Fugitive dust control with pipe cyclone
CASE STUDIES
Particle Science and
Technology Laboratory
Crystallization
i) various types of agitators/agitation
speeds/profiles for obtaining specific particle size
distribution (PSD)

ii) characteristic cooling profiles for generating
particle size requirements

iii) Impact of heat dissipation on PSD

iv) Use of ultrasonic waves for obtaining uniform
PSD
EARLITER
DISCUSSIONS
Particle Science and
Technology Laboratory

Control of PSD

addition of antisolvent on PSD
spraying high velocity jet on PSD.
Usage of high frequency dryers to obtain
uniform PSD.
Usage of alphine air jet milling to
optimise/control PSD.
EARLITER
DISCUSSIONS
Particle Science and
Technology Laboratory
Chargeability/Zeta potential

Effect of charge on PSD, dispersion
Charge dissipation techniques, especially
usage of photo-deioniser for charge
dissipation for powdered products.
formation of agglomeration due to
chargeability
accumulation of charge during storage
and transportation
EARLITER
DISCUSSIONS
Particle Science and
Technology Laboratory

a) Containment of micronized /fine milled Powders
i) in powder processing areas
ii) during storage

b) Effect of repeating milling/size reduction on
profile of particle size distribution. Illustrate with
Comminution functions such as selection and
breakage function.

c) Control of Particle shape during unit operations
and particle shape measuring technologies.
EARLITER
DISCUSSIONS
Particle Science and
Technology Laboratory
Particle Manufacture
By Breakdown
GRINDING (Solids)

SPRAYING (Liquids)
Particle Science and
Technology Laboratory
Particle Design
By Growth
PRECIPITATION
CRYSTALLISATION
POYMERISATION
CHEMICAL VAPOUR
DECOMPOSITION
From
LIQUID
From
GAS
GRANULATION
SINTERING
From
SOLIDS