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Powder characteristics
Single particle characteristics

Particle systems

Primary chemical composition

Distribution of chemical
compostion
Impurity composition and distribution
Distribution of
impurities
Phase composition (Mineralogy)
Distribution of phase
compositions
Crystal defects
Porosity and pore
structure
Porosity, pore structure
Particle size
distribution
Size
Particle shape distribution
Shape
Bulk density
Density
Specific surface area
Specific surface area
Bulk composition
Agglomeration state
The underlined properties are routinely determined

Particle size

Frequently used particle sizes

1.The Stokes diameter is the diameter of a
spherical particle that has the same density and
settling velocity as the particle (laminar flow)

Definition of diameters

Equivalent sphere
(volume) diameter
Sieve diameter (minimum
mesh size through which
the particle will fall)

Minimum, maximum
diameters

2.The aerodynamic diameter is the diameter of

the water droplet that has the same settling
velocity in air.
3.The volume diameter is the diameter of a
sphere having the same volume as the particle.
4.The surface-volume diameter is the diameter
of a sphere having the same surface-to-volume
ratio as the particle.

5.The sieve diameter is the width of the

minimum square aperture through which the
Chord length in particular particle will pass.
reference direction
6.The Feret's diameter is the mean value of the
distance between parallel lines tangent to the
outline of the particle.

Aspect ratio: longest diameter/shortest

Particle size measurements: Light diffraction I

Suspension

Laser

When a light beam illuminates an aerosol, some light is

transmitted through a suspension, while some is absorbed
and some is scattered by the particles. The light scattered
by a particle is a function of its size, shape, refractive
index and the wavelength of the incident beam.
For particles with refractive index nP , wiith a diameter R
smaller than the wavelength of the laser light and
suspended in a medium with refractive index nM, (n= nP / nM)
the intensity Is scattered at angle can be described by
the equation given by Raleigh:
2

Is ( ) 1 16 4 R 6 n 2 1
2
2
4 2
1 cos
I0
r 2
n 2

Laserlight

Detector
QuickTime and a
TIFF (Uncompressed) decompressor
are needed to see this picture.

For particles larger than the wavelenght of light the

Raleigh equation does not hold anymore and the Mie
scattering theory has to be applied.
Each particle gives a Fraunhofer diffraction pattern which
overlap.

Powder characterisation

Particle size measurements: Light diffraction II

Intensity

+
0
Scattered intensity as function of
scattering angle for three
individual particles (red < blue <
green)

0
Sum of the scattered intensities
shown on the left.

Particle size measurements: Light diffraction III

Fraunhofer diffraction pattern
(2.5x) of a particle of unknown
size. The position of the center
of the dark areas is related to
particle size a by the following
equation

Fraunhofer diffraction aureole

around the sun caused from arctic
haze aerosol

Particle size distributions I

100%

monodispersed

50%

polydispersed

10%
1

10

100

size (mm)

Type of particle size distributions

Representation of particle size distributions

(Reed, 1995)

Mean particle size

Definition of different arithmetic and geometric mean particle diameters
(mathematical function of the size distribution function unknown):
On a number of particle basis:
length diameter

dL

Arithmetic mean

Geometric mean

ln d

N i di
N

surface diameter

dS

N d
N
i

2
i

volume diameter

dV

N d
N
i

3
i

N ln d
N
i

Ni = Number of particles in class i

di = mean diameter of particles in class i
If the fractional size distribution is given on a mass basis, the following equation
allows to convert it to a number basis distribution:

Ni

Mi
V di 3

Ni = Number of particles in class i

Mi = Mass of the particles in class i
= density of particles
v= volume shape factor
di = mean diameter of particles in class i

Particle shape
A dimensionless combination of different average diameters of a distribution of
particles is called a shape factor. Shape factors have three functions:
-Proportionality factors between different particle size determination methods
-Conversion factors for expressing results in terms of an equivalent sphere
dimension
-Transformations of the measured particle diameter into particle surface and volume
respectively.
The most common shape factor is the aspect ratio e.g. the ratio between the largest
and the smallest diameter of a particle.
The volume shape factor is defined as:

Vt
Ni di 3

Vt = Total volume of the particles

Ni = Number of particles in class i
di = mean diameter of particles in class i

Agglomeration states I
Agglomeration state:

Well dispersed

hard or soft agglomerated

Agglomerated powders should be dispersed by ultrasonic treatment or milling before use.

Hard agglomerates in alumina

produced by the Bayer-process.
(Reed,1995)

As recieved zirconia powder

with soft agglomerates.

Zirconia powder shown in the

center image after dispersion.

Particle density I
Density

openporosity(Vop)

closedporosity(Vcp)

Densities:
ultimate density: M/Vs
apparent density: M/(Vs + Vcp)
bulk density: M/(Vs + Vcp + Vop)
M: particle mass (empty pores)
Vs : volume of solid

Pycnometry
This method allows to measure
the apparent density.
(Reed, 1995)

Powder characterisation

Particle density II
The mercury injection porosimeter allows to measure the open
porosity
The volume of mercury (contact angle
with most solids = 140) forced into
the pores of the solid is mesured as
a function of pressure. The pore size
distribution is calculated using the
relationship between applied pressure
and the radius of the pore which can
be filled by this pressure

2 cos
p
r
= wetting angle (140 for most solids)
= surface tension mercury - sample
r = pore radius
(Reed, 1995)

Particle density III

a

Cumulative pore volume curve as function of

pore size. Hysteresis is usually obeserved.
This reflects some of the mercury being
permanently trapped in ink bottle pores.
The volume of the latter is given by the
residual Hg entrapped when Hg pressure is
reduced to atmospheric presssure.

Cumulative pore volumes for alumina

powder containing agglomerate of a)
porous particles b) non-porous
particles.

Three ink-bottle pores

Specific surface area

Specific surfaces are determined by
measuring the amount of nitrogen gas
adsorbed at the surface (BET method)
Assumption: only one layer of nitrogen is
adsorbed. The specific surface is given
by

N A VM AM
S
V Mol M s

MeasuringsetupforBET(Bernauer,EmmetandTeller)
measurements.

NA:Avogadrosnumber
VM:adsorbedgasvolume
AM:areaoccupiedbyoneadsorbatemolecule
VMol:volumeofonemolofgasatstandardP,T
Ms:massofthesample
The solid must be free from previously
adsorbed gases and vapours. Evacuation
at 10-4 Torr for several hours is
necessary. It is possible to heat the
solid (100-400c).

Powder characterisation

Powder specifications I
Specifications for three Bayer process aluminas

Powder specifications II
Specifications for three barium titanate powders

Powder segregation I

Progress of segregation (a-c)

that results after bidisperse
color-coded particles are
poured into a silo. A sharp
reduction of segregation is
observed when a small volume
fraction of fluid is added which
introduces capillary bridges
between particles (d).
http://physics.clarku.edu/~akudrolli/w
et-seg.html

Powder segregation II
Simulation of particle size segregation during vibration. Interestingly the large
particles move upward = Brazilian nut effect! (http://www.granular.com/POWDER/tour.html)

Langmuir isotherm II
The Langmuir isotherm can be tested in arranging it in a linear form:

KPa KPa

KPa
KPa
KPa

can hardly be determined, but the volume v of gas taken up by the sample can be
measured. The ratio between the volume of the adsorbed gas (v) and the maximum
volume uptake (V) assumed to correspond to a total monolayer coverage is proportional
to the surface coverage.
so

v
P P
1
a a
V
v V KV

AplotofP/vagainstPis
linear.
Theinterceptallowsto
determineKatconstantT.

Microcrystalline cellulose is one of the most useful filler for direct compression.
Cellulose in general consists of an amorphous part and a crystalline part, which
can exist in two
polymorphic forms: cellulose I and cellulose II. UICEL (University of Iowa
cellulose)
is a cellulose II product and can be obtained by mercerization (chemical
treatment with sodium hydroxide) from Avicel PH102, a microcrystalline
cellulose, which contains the cellulose I polymorph. X-ray measurements of the
two substances confirmed the different polymorphic forms and demonstrated a
higher degree of crystallinity for Avicel PH102(73%) than for UICEL (64%).

Cellulose exists in four major crystal modifications, cellulose I, II, III and IV. The
polymorphic forms can be interconverted according to figure 3 mostly by certain
chemical and thermal treatments

Figure 3: Interconversion of the polymorphs of cellulose.

Pengaruh density granul terhadap kekerasan tablet