POWDER TECHNOLOGY
POWDER FLOW PROPERTIES
• Powder flowability is defined as ease with which a powder will flow under a set of conditions
• Pharmaceutical powders may be classified as free-flowing or cohesive (non-free flowing/sticky)
• Flow properties are significantly affected by changes in particle size, density, shape, electrostatic
charge and adsorbed moisture, which may arise from processing or formulation.
• Flow properties depend on frictional force and force of cohesion between one powder particle and
another. Thus, an in-depth knowledge of the flow properties of powders is essential for an efficient
mixing and tabletting process
POWDER FLOW PROPERTIES CONT’
• Many common manufacturing problems are attributed to Powder flow.
a) Volumetric filling: Powder transfer through large equipments such as hoppers
b) Uneven powder flow leading to excess entrapped air within Powders resulting in
capping or lamination
c) Uneven powder flow leading to increase particle’s friction with die wall causing
lubrication problems and increase dust contamination risks during powder transfer.
POWDER FLOW PROPERTIES CONT’
d. Powder storage, which for example result in Caking tendencies within a vial or
bag after transport or on storage.
e. Separation of small quantity of the powder from the bulk-specifically just before
the formulation of individual doses such as during tableting, encapsulation and
vial filling which affects the weight uniformity of the dose
POWDER PROPERTIES
A. PARTICLE SIZE
• Frictional and cohesive forces (resistance to flow) are increased as the particle size is
reduced. Very fine particles don't flow as large particles
• In general, particles in the size range of 250-2000 micron flow freely if the shape is
agreeable.
• Particles in the size range of 75-250 micron may flow freely or cause problems, depending
on shape and other factors. With particles less than 100 micron in size, flow is a problem.
POWDER PROPERTIES CONT’
B. PARTICLE SHAPE
Rough/Flaky/Dendritic, irregular particles present more points of interparticulate contact
than smooth spherical Particles thus spherical particles have better flow properties than
irregular particles
C. MOISTURE CONTENT
Drying the powders will reduce the cohesiveness
POWDER PROPERTIES CONT’
D. SURFACE PROPERTIES i.e. Electrostatic charge
The presence of electrostatic forces can add to interparticulate attractions and promote
closer packing, resulting in increased cohesion between particles resulting in reduced
flow rate
E. PARTICLE SIZE DISTRIBUTION
Void spaces between coarse particles may become filled with finer particles in a
powder with a wide size range, resulting in more closely packed cohesive powder.
F. POROSITY
Solid particles from grinding, milling, leaching process often exhibit cracks, cavities and
holes (collectively termed as pores) within the structure.
Porosity is a measure of void volume in a material and is expressed as a fraction or a
percentage of the total volume (bulk volume)
Void volume = bulk volume – true volume
G. DENSITY
Because powders flow under the influence of gravity, dense particles are generally less
cohesive than less dense particles of the same size and shape
• There are three density expressions usually associated with powders
a) True/ absolute density: excludes the volume of pores and interparticulate spaces
b) Envelope/ apparent density: includes the pore volume but exclude the particle
spaces
c) Bulk density: includes the pore volume and interparticulate spaces
• Bulk density is of great importance for capsule filling, tablet compressibility and for the
homogeneity of formulation in which there are large difference in drug and excipient
densities.
• Apparent bulk density (g/ml) is determined by pouring pre-sieved bulk drug into a
graduated cylinder via a large funnel and measuring the volume and weight .
• Powders with low apparent density and large bulk volume are light powders, and those
with high apparent density and small bulk volume are heavy powders.
CHARACTERIZATION OF POWDER FLOW
• Four commonly methods of characterizing powder in pharmaceutical industries
include:
a) Angle of repose
b) Compressibility index or Hausner ratio
c) Flow rate through an orifice
d) Shear cell
ANGLE OF REPOSE
• The sample is poured onto the horizontal surface and the angle of the resulting pyramid
is measured.
• The user normally selects the funnel orifice through which the powder flows slowly
and reasonably constantly.
• The angle of repose can be determined experimentally by allowing a powder to flow
through a funnel and fall freely onto a surface.
• The height and diameter of the resulting cone is measured.
PROCEDURE
• Take a certain amount of powder and form the angle of repose on a fixed base, the base should
be free of vibration
• Vary the height of the funnel to carefully build up a symmetrical cone powder. Care should be
taken to avoid vibration as the funnel is moved.
• The funnel height should be maintained approximately 2-4 cm from the top of the powder pile
as its us being formed in order to minimise the impact of falling powder on the tip of the cone.
• Determine the angle of repose by measuring the height of the cone of the powder and
calculating the angle of repose from the following equation:
FLOW PROPERTY AND CORRESPONDING
ANGLE OF REPOSE
FLOW PROPERTY ANGLE OF REPOSE (DEGREES)
Excellent 25-30
Good 31-35
Fair- aid not needed 36-40
Passable – May hang up 41-45
Poor- must agitate, vibrate 46-55
Very poor 56-65
Very, very poor > 66
COMPRESSIBILITY INDEX AND HAUSNER
RATIO
• The basic procedure is to measure the apparent volume, , and final tapped volume/true
volume, , of the material after tapping the material until no further volume changes
occur.
• A volume of powder is filled into a graduated glass cylinder and repeatedly tapped for a
known duration. The volume of powder after tapping is measure
• The compressibility index and the hausner ratio are calculated as follows:
• Alternatively, the compressibility index maybe calculated by using the measured values
for bulk density and tapped density as follows:
SCALE OF FLOWABILITY
COMPRESSIBILITY FLOW CHARACTER HAUSNER RATIO
INDEX (%)
Excellent 1.00 – 1.11
11-15
11-15 Good
Good 1.12
1.12 –
– 1.18
1.18
16-20
16-20 Fair
Fair 1.19
1.19 –
– 1.25
1.25
21-25
21-25 Passable
Passable 1.26
1.26 –
– 1.34
1.34
26-31 Poor 1.35 – 1.45
26-31 Poor 1.35 – 1.45
32-37 Very poor 1.46 – 1.59
32-37 Very poor 1.46 – 1.59
> 38 Very, very poor > 1.60
> 38 Very, very poor > 1.60
FLOW RATE THROUGH AN ORIFICE
• The flow rate through an orifice has is generally measured as the mass per time flowing
from any number of types of containers (cylinders, funnels, hoppers)
• Flow rate is classified on the basis of three variables
a) Type of container: Cylinders, Funnels, Hoppers from production equipment
b) The size and shape of orifice used
c) Method of measuring powder flow rate: Flow rate can be measured continuously (
use an electronic balance attached to a recording device) or discrete samples i.e.
the time it takes for a 100g of powder to pass through an orifice
Suitable for materials that have capacity to flow
IMPROVEMENT OF POWDER FLOWABILITY
A. 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 flowability by removing a
proportion of the fine particle fraction or by increasing the proportion of coarser
particle’s such as occurs in granulation.
B. 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 cohesive and have a greater tendency to
interlock than smooth surfaced particles. This can be altered by control of production
methods such as crystallization
C. Alteration of Surface Forces
• Reduction of electrostatic charges can improve flowability.
• Electrostatic charges can be reduced by altering process conditions to reduce frictional
contacts.
• Moisture content of particle greatly affects powder’s flowability.
• Adsorbed surface moisture films tend to increase bulk density and reduce porosity.
• Drying the particles will reduce the cohesiveness and improve the flow.
• Hygroscopic powder’s stored and processed under low humidity conditions.
D. Formulation additives (flow activators)
• Flow activators are commonly referred as glidants.
• Flow activators improve the flowability of powders by reducing adhesion and cohesion.
• Examples:. Talc, maize starch and magnesium stearate
E. Use of vibration assisted hoppers and force feeder
• They are attached to electric motors which provide the vibrational energy
EQUIPMENT FOR MILLING
• HAMMER MILL
FLUID ENERGY MILL
COLLOID MILL
END RUNNER MILL
CUTTER MILL
VIBRATION/BALL MILL
