Derived properties of Powders

Porosity
Suppose a powder, is placed in a graduated cylinder:
• the total volume occupied is known as the bulk volume Vb .
• bulk volume = true volume + volume of spaces between particles.
The volume of the spaces, the void volume, V = Vb - Vp
• Vp is the true volume of particles.
• The porosity or voids ε of powder is determined as the ratio of void volume
to bulk volume.
Vb – Vp Vp
Porosity (ε) = = 1-
Vb Vb
• Porosity is frequently expressed
in percent, ε x 100
 Porosity
 A sample of calcium oxide powder with a true density of 3.203 and weighing
131.3g was found to have a bulk volume of 82 cm3 when placed in a 100-ml
graduated cylinder. Calculate the porosity ??
 Packing arrangement
 Powder beds of uniform-sized spheres can assume either of two ideal
packing arrangements: (a) closest or rhombohedral and (b) most open,
loosest, or cubic packing.
 The theoretical porosity of a powder consisting of uniform spheres in
closest packing is 26% and for loosest packing is 48%.
 The particles in real powders are neither spherical in shape nor uniform in
size. Thus, the particles of ordinary powders may have any arrangement
intermediate between the two ideal packings.
 If the particles are of greatly different sizes, however, the smaller ones
may shift between the larger ones to give porosities below the theoretical
minimum of 26%.
 In powders containing f lo cculates or aggregates, which lead to the
formation of bridges and arches in the packing, the porosity may be above
the theoretical maximum of 48%.
 Density
• Density is defined as weight per unit volume (W/V).
• During tapping, particles gradually pack more efficiently, the powder
volume decreases and the tapped density increases.
True density: The true density or absolute density
of a sample excludes the volume of the pores
and voids within the powder sample.
Bulk density: The bulk density value includes the
volume of all of the pores within the powder
sample.
 Bulkiness
Bulkiness = Specific bulk volume = reciprocal of bulk density
It is an important consideration in the packaging of powders.
Bulkiness increases with a decrease in particle size.
In mixture of materials of different sizes, the smaller particles sift between
the larger ones and tend to reduce bulkiness.
 Flow properties
 Powders may be free-flowing or cohesive (sticky).
 Many common manufacturing problems are attributes to powder flow.
 Powder transfer through large equipment such as hopper.
 Uneven powder f lo w  excess entrapped air within powders 
capping or lamination.
 Separation of small quantity of the powder from the bulk- specif ically
just before the creation of individual doses such as during tableting,
encapsulation and vial f illing which affect the weight uniformity of the
dose (under or over dosage).
 Evaluation of flowability
Carr’s Compressibility Index
 A volume of powder is f il led into a graduated glass cylinder and
repeatedly tapped for a known duration. The volume of powder after
tapping is measured.
% Compressibility = (Tapped density – Bulk density/Tapped density)*100

% COMPRESSIBILITY FLOW DESCRIPTION

5 – 15 Excellent
12 – 16 Good
18 – 21 Fair
23 – 28 Poor
28 – 35 Poor
35 – 38 Very Poor
> 40 Extremely Poor
 Evaluation of flowability
Hausner Ratio
Hausner Ratio = Tapped Density / Bulk Density

Hausner ratio is related to interparticle friction:

 Value less than 1 .25 indicates good f lo w (the powder with low
interparticle friction, such as coarse spheres).
 Value greater than 1.5 indicates poor f lo w (more cohesive, less free-
flowing powders such as flakes).
 Between 1.25 and 1.5, added glidant normally improves flow.
 > 1.5 added glidant doesn’t improve flow.
HAUSNER RATIO TYPE OF FLOW

Less than 1.25 Good Flow

1.25 – 1.5 Moderate

More than 1.5 Poor Flow

 Evaluation of flowability
The Angle of Repose
The frictional forces in a loose powder can be measured
by the angle of repose α.
α = the maximum angle possible between the surface
of a pile of powder and horizontal plane, which could be
correlated with coeff ic ient of friction μ between the
particles:
tan α = μ
tan α = h / r
r=d/2
α = tan-1 (H / R)

The rougher and more irregular the surface of the particles, the higher will be the angle of
repose.
ANGLE OF TYPE OF FLOW
 The sample is poured onto a horizontal
REPOSE surface and the angle of the resulting
< 25 Excellent pyramid is measured. The user normally
selects the funnel orif ice through which
25 – 30 Good
the powder f lows slowly and reasonably
30 – 40 Passable
constantly.
> 40 Very Poor
 Improvement of powder flow property
Alteration of Particle’s size & Distribution

There is certain particle size at which powder’s flow ability is optimum.

Coarse particles are more preferred than fine ones as they are less cohesive.

The size distribution can also be altered to improve f lowability by removing a

proportion of the fine particle fraction or by increasing the proportion of coarser
particles, such as occurs in granulation.
Alteration of Particle Shape & texture

Particle’s Shape:
Generally, more spherical particles have better
flow properties than more irregular particles.
Spherical particles are obtained by spray drying,
or by temperature cycling crystallization.

Particle's texture:
Particles with very rough surfaces will be more
cohes ive and h ave a greater tendency to
 Improvement of powder flow property
Alteration of Surface Forces
-Reduction of electrostatic charges can improve powder flowability.
• Electrostatic charges can be reduced by altering process conditions.
-Moisture content of particle greatly affects powder’s flowability.
• Drying the particles will reduce the cohesiveness and improve the flow.

Formulation additives ( Flow activators)

- Flow activators are commonly referred as glidants.
- Flow activators improve the f lowability of powders by reducing adhesion and
cohesion (e.g. talc, maize starch and magnesium stearate)
Particle shape and specific surface
 Particle Shape
 Particle shape also has inf lu ence on surface area, f low properties,
packing and compaction of the particles.

 Spherical particles have minimum surface area and better f lo w

properties.

 Techniques of determination are:

 Microscopy
 Light scattering
 Specific surface area

 Surface area of a powder can be calculated using particle size data obtained
from any suitable method.

 Specif ic surface area i.e. surface area per unit weight (Sw) or unit volume (Sv)
can be estimated as follows:
 DETERMINATION of surface area
 Adsorption method:
 Surface area is most commonly determined based on Brunauer-
Emmett-Teller (BET) theory of adsorption.

 Most substances adsorb a monomolecular layer of gas under certain

conditions of partial pressure of gas and temperature.

 The adsorption process is carried out at liquid nitrogen temperatures

-196C̊.

 Once surface adsorption has reached equilibrium, the sample is

heated at RT and Nitrogen gas is desorbed. Its volume is measured.
 Air Permeability method:

 Powder is packed in sample holder and air is allowed to pass through

the capillaries at constant pressure
 Resistance is created as air passes through samples thus causing
pressure drop.
 Greater the surface area greater the resistance
 Air permeability is inversely proportional to the surface area