Comminution

Introduction
• The operation which involves the reduction of
particle size from larger to smaller particles.
• also called size reduction, Milling, grinding.
• This size-reduction operation can be divided
into two major categories depending on
whether the material is a solid or a liquid. If it
is solid, the operations are called milling, if it is
liquid, emulsification or atomization.
 Reasons and importance
• Increase surface area which increase the solubility, and
• dissolution rate and bioavailability.

• Improvement and increasing the drying rate of particles.

• Improve mixing of materials especially powders.

• Improve flowability of materials in tablet machine.

• Pharmaceutical suspensions require fine particle size.

• To reduce grittiness of ophthalmic and topical products

• To improve texture of ointment, creams and pastes.

• Lubricant has a fine powder in order to cover more surface area.
• The extraction process is increased if the size is reduced
 Factors affecting size reduction

1. Hardness and toughness

 ↑ hardness → difficult is the size reduction
2. Abrasiveness
 Abrasive material → chances of contamination with metal worn from the
grinding mill
3. Stickiness
 ↑stickiness → ↑adherence to the grinding surface and choking of the mesh.
5. Softening with temp
 Many of the size reduction process generate heat. This may cause the softening
of substance.
6. Structure
 Several substances have lines of weakness along which the material fracture in
peaces.
7. Moisture contents
 Material should be dry or wet but not damp
8. Feed size
 Feed size should be optimum to avoid choking of the mill.
Size analysis of a powder
Microscopy
• The most and simple direct method .
• By means of a calibrated micrometer eyepiece
• The hair line of the eye piece is moved by the micrometer to one edge of the
particles, and the reading on the micrometer is recorded. The hairline is then
moved to the opposite edge of the particle being measured, the micrometer is
read.
• The difference in the reading is the size of the particle.
• Lower limit is 0.4 μm. However, with latest lenses this may be extended to 0.1 μm.
• This method is used for particle size analysis in suspensions, aerosols and
emulsions.
• Shape can be seen.
• Agglomerates can be seen and avoided while counting.
• Precise measurement because of particles static position.
• Only 2 dimentional measurement
• Slow and tidious
Sieving
• Cheap, simple and rapid
• Sample of powder through a series of successively smaller sieves. In
other words, a number of sieves that fit into each other in a frame
(i.e. a rack of sieves). The coarsest sieve is placed on top and the
finest one at the bottom. Powder is passed successively over finer
sieves and a series of fractions obtained.
• The percentage of fraction left on each sieve is calculated, which give
a particle size distribution.
• Sieving does not give accurate results.
• NOTE: Sieve is a mesh made up of wire or nylon or a plate perforated
with holes. The one used for particle size analysis is of wire type.
• Mesh number: The mesh number system is a measure of how many
openings there are per linear inch in a screen.
• If particls are wet, the pores of the sieves can get clogged with
particles and sieving would be improper.
• Since the sieves are shaken, the particles collide with each other and
there are chances of further size reduction which can lead to errors.
Sedimentation
• This is based on the rate of sedimentation.
• The powder is dispersed in the liquid contained in a tall vessel
(Andreasen apparatus).
• 10ml sample are withdrawn at predetermined times form a
known depth bellow the surface and determined by
evaporating the liquid and weighing the residue, in order to
calculate the range of particle sizes present in each sample.
• Stokes’s equation is used. This is only applicable in dilute
dispersions where the concentration of solid is less than 2%
w/w.

• Dst= stokes diameter, x(h)= distance of all in time, p= particles density, p0=dispersion medium density, n=viscosity of medium, g= gravitational
accelaration

• In one of the methods the settlement rate is increased by using

a centrifuge. Calculation of the results is by stokes’s law, with an
appropriate factor to indicate the number of times the
centrifugal force is greater than the gravitational force.
• Reliable as a whole of the sample is screened. But is a rough
estimate of size in each layer.
Andreasen apparatus
• LASER particle size analyzer :
• This depends on the laser ray diffraction by
the particle. This is suitable for online particle
size determination. When the process is going
on the particle size can be measured by
LASER diffraction technique without the need
to halt the manufacturing process.
• Advantages: It is reliable method and also less
time-consuming.
Conductivity method
• One of the more recent particle size analysis procedure
depending upon conductivity measurement is Coulter
Counter.
• In which the particles are suspended in an electrically
conductive fluid.
• The suspension flows through a suitable aperture with
an immersed electrode on either side and the particle
concentration is arranged so that only one particle
travels through the aperture at a time.
• As the particle passes through the aperture, some
electrolyte is displaced and changes the resistance
between the electrodes which causes a pulse in the
voltage. The magnitude of the pulse will be proportional
to the size of the particles.
• Reliable and faster.
• Expensive
Particle size distribution
• The shape of the particle is irregular, and the size of particles
varies within the range of the largest and smallest particles.
• No method has been developed to express the exact size and
shape of a particle mixture. However, statistical methods have
been developed to express the size of an irregular particle in
terms of a single dimension reffered to as its diameter.

• Similarly there are various methods for representation of

particle size distribution.
• The most precise method of data presentation is tabular form.
• Other methods are bar graph, or histogram of the frequency
as a function of particle size .
• Size distribution data are commonly presented graphically
because a graph is more concise and permit easy
visualization.
 Theories
• Rittinger’s theory

• It suggests that energy required in a size reduction process is

proportional to the new surface area produced.

• Kick’s theory

• Kick’s theory states that the energy used in deforming (or

• fracturing) a set of particles of equivalent shape is proportional to
the ratio of change of size.
How much energy is needed to crush or grind particles into smaller
particles. It says energy depends on how much size is reduced as a ratio
not the actual size of the particles. e.g. crushing a substance to ½ of its
size need same energy regardless of how big or small size.
MECHANISMS OF SIZE REDUCTION
• There are four main methods of effecting size reduction,
involving different mechanisms
• Cutting:
• as the name implies, the material is cut by means of a sharp
blades
Compression:
• in this the material is crushed by application of pressure.
Impact:
• occurs when the material is more or less stationary and is hit
by an object moving at high speed or when the moving
particle strikes a stationary surface. In either case the material
shatters to smaller pieces.
Attrition:
• In attrition the material is subjected to pressure as in
compression, but the surfaces are moving relative to each
other, resulting in shear forces which break the particles.
Pistle and
mortar
TYPES OF PHARMACEUTICAL MILLS
• Coarse milling: ˃20 Mesh
• Intermediate milling: 20-200 mesh
• Fine milling: ˂200 mesh
• A mill can operate in more than one
mechanism.
• It has three basic parts
1. Feed channel
2. Mean of grinding
3. Discharge channel
• The rate of feed should be equal to the rate of
discharge.
• Mostly gravitational force is sufficient for
discharge from bottom of the mill. However for
ultra fine particles, air or inert gas is
introduced to carry the milled product with it.
• The mills where the material is reduced to the
desired size by passing once through the mill
are called open circuit milling.
• The mills where the larger particles are
redirected to the grinding chamber until
reduced to smaller sizes are called closed
circuit milling.
 Cutter mill
• Construction and working principle: The equipment has two parts
• – one is rotor and another part is the casing. Stationary knives are
• fitted on the casing and rotating knives are fitted on the rotor. Feed
• enters through the top hopper. The rotor rotates and both stationary
• and rotating knives cut the material into pieces. The lower part
• consists of a screen, so that material is retained in the mill until
• sufficient degree of size reduction has been effected.

• Applications:

• This method is used to obtain coarse degree of size reduction of soft

• materials.

• Applied in size reduction of roots, peels or woods, prior to

• extraction.
Hammer Mill
Design features:
1. feed inlet at top or center
2. Milling chamber, which contain
3. A rotor having swinging hammers
4. The plates at the inner surface of the casing
5. Perforated metal screen (forms the lower portion of the casing)
Mechanism of size reduction
Impact of the hammers against the plates in the internal wall of the mill.
Operation
• Material is fed into the mill's chamber from top or center.
• The material is struck by swinging hammers which are attached to a shaft which
rotates at high speed inside the chamber. The material is crushed or shattered by
the repeated hammer impacts, and collisions with the walls of the grinding
chamber.
• Perforated metal screens, covering the discharge opening of the mill retains
coarse materials for further grinding while allowing the small sized materials to
pass as finished product.
• Hammer speed 7600rpm/min at which every material behave as brittle.
• Hammers may be either blunt or cutting edges.
• Brittle material is best reduced by blunt hammers, while fibrous material by
cutting edges.
• Size of particles are controlled by hammer speed and the size and type of screen.
Advantages
• It is rapid in action, and is capable of grinding many different
types of materials.
• No surface moves against each other, so that there is little
contamination of the product with metal abraded from the
mill.

Disadvantages
• The high speed of operation causes generation of heat that
may affect thermolabile materials or drugs containing gum,
fats or resins.
• The rate of feed must be controlled, to avoid chocking of the
mill.
Application
• Milling of barks, leaves, roots, crystals, filter cakes.
Ball mill
 Ball mill
• Construction

• The ball mill consists of a hollow cylinder rotated on its horizontal axis. Inside
• the cylinder balls or pebbles are placed.

• Cylinder:

• Cylinder may be made up of metal, porcelain or rubber.

• Diameter of the cylinder ranges from 1 to 3 m in pharmaceutical practice.

• Balls:

• Balls occupy about 30 to 50% of the volume of the cylinder.

• Diameter of the balls depends on the feed size and diameter of the cylinder.
• The diameter of balls ranges from 2 cm to 15 cm. OR…. 75 mm, 150 mm, 20 mm.

• Balls may be of metal, porcelain or pebbles.

• Working Principle: Larger particles are fed through an opening of the
• cylinder. The opening is closed. The cylinder is rotated at the critical
• speed of ball mill (Generally it is 0.5 cycles per seconds (cps)). The
• optimum size reduction in a ball mill depends o the following factors:

• Feed quantity: Too much feed will produce cushioning effect and too
• little feed will produce loss of efficiency of the mill.

• Speed of rotation of the cylinder: At low speed the mass of balls will
• slide or roll over each other and only a negligible amount of size
• reduction will take place.

• At high speeds, balls will be thrown out to the wall of the cylinder due
• to centrifugal force and no grinding will occur.
 Advantages:

• Capable of grinding wide variety of material.

• It can be used in a completely enclosed form,
which makes it suitable for toxic materials.
• It produces very fine powders. Ball mills are
effective grinding systems in the general range
of 500 microns down to 5 microns
• Suitable for wet and dry milling.
 Disadvantages:

• Wear and tear may occur which may results in

product contamination.
• Soft or sticky material may cause problem by
caking on the side walls or holding the balls.
• It makes a lot of noise specially in case of
metallic material of construction.
Colloid Mill
 Colloid Mill /homogenizers…..for suspension and emulsions…..not
for dry materials

• Colloid mill is used to reduce the particle size of a solid in suspension, or to

reduce the droplet size of a liquid suspended in another liquid.
Mechanism of size reduction
• This is done by applying high levels of hydraulic shear to the process liquid. It is
frequently used to increase the stability of suspensions and emulsions.
Design features:
• Consist of a high speed rotor (3000-20000rpm) and stator.
• The rotor and stator are cone shaped, and have three stages of increasingly
grooves. The grooves change directions in each stage for increased turbulence.
• The stator can be adjusted to obtain the desired gap setting between the rotor
and stator.
• material is fed from top through the hopper upon the rotor, the centrifugal force
throws the material across the rotor on to the stator. The hydraulic shearing force
(in the narrow gap b/w rotor and stator) tends the particles to break in to smaller
ones.
• The milled material is discharged through an outlet and may be recycled.
 ROLLER MILL
•
• Method of size reduction: Compression
•
• Construction and working principle:
• The roller mill has two cylindrical rolls of stone or metal, mounted horizontally,
which are capable of rotating on their longitudinal axes. One roll is rotated
directly using a motor and the other rotates freely. When material is placed
above the rolls it is drawn in through the nip and the second roll is rotated b y
friction.
• Diameter of the rolls: Few centimeter up to several meters
• The gap between the roll may be adjusted to control the degree of size
reduction.
•
• Applications:
• Used for crushing or cracking seeds prior to extraction of fixed oils or bruising
soft tissues (often after cutting) to aid solvent penetration.
•
Fluid Energy Mill/micronizer
• Principle
• It works mainly on the principle of attrition and impact.
• Basic parts
• The main basic parts present in the fluidized energy mill are
as follows
• The inlet by which the solid material is introduced into the
chamber which is made of stainless steel.
• The nozzles by which the air and the inert gas is introduced
into the chamber at high pressure.
• The classifier from which the fine reduced particles are
collected
• Construction
• It consists of a loop of pipe which has a
diameter of 20 to 200 mm, depending on the
overall height of the loop, which may be up to
about 2 m.
• There is an inlet for the feed and a series of
nozzles for the inlet of air or an inert gas.
• It also has an outlet with a classifier which
allows the air to escape but prevents to pass
until they become sufficiently fine.
• Working
• In the operation of a fluid energy mill, gas of high
energy content is introduced into a pulverizing chamber.
The air or inert gas is introduced with a very high
pressure (100 to 150 psi) through the nozzle. Solids are
introduced into air stream through the inlet. Due to the
high degree of turbulence, impact and attritional forces
occurs between the particles.
• The fine particles are collected through a classifier. Fluid
energy mill reduce the particles to 1 to 20 micron. To
get a very fine powder even up to 5 micron the material
is pretreated to reduce the particle size to the order of
100 mesh and then passed through fluid energy mill.
• A size-reduction unit depending for its action
on collisions between the particles, the energy
being supplied by a compressed fluid, (e.g., air
or steam) that enters the grinding chamber at
high speed. Such mills will give a product of 5
micron or less.
• ADVANTAGES
• Air needed is free.
• Large range of sizes available.
• The mill is used to grind the materials to fine powder.
• The particle size of the powder can be controlled due
to the use of a classifier.
• There is no wear of the mill and hence there is no
contamination of the product.
• It is useful for grinding heat sensitive substances such
as sulphonamides, vitamins and antibodies.
• Homogeneous blend.
• DISADVANTAGES
• Energy consuming.
• High head space.
• Avoid coarse materials into the chamber.
• The fed device may be clogged with the clump materials.
• Special feeding devices should be provided for the
feeding of the materials.
• One of the problems encountered with the use of
compressed air is the generation of static electricity.
• Material recovered in the collection bags is difficult or
impossible to remove by the normal blow back
procedures.
 Types
There are two main classes of pulverizers
Air swept pulverizer
Air impact pulverizer
Air swept pulverizers use air to transport particles to the
pulverizing section of the apparatus. Air impact
pulverizers use high speed air to pulverization of the
particles.
The products from both air swept and air impact
pulverizers produces oversize particles and no need of
further sieving or classifying.

An air swept pulverizer primarily uses air to classify and separate

particles based on size, while an air impact pulverizer uses a high-
impact force to grind materials into fine powder, with air also
playing a role in particle size control and separation;
End runner mill
• Principle :shear and crushing
• Construction :
• The end-runner mill consists of a weighted pestle
mounted eccentrically in a ceramic, granite or metal
mortar, which is rotated by a motor. The pestle rotates by
friction and is free to rise and fall in the mortar so that its
grinding action involves both impact and shear, the
material being crushed and rubbed between it and the
rotating mortar.
• Spring-loaded scrapers ensure that material is constantly
returned to the grinding area and at the end of the
operation the pestle can be swung clear of the mortar to
facilitate emptying and cleaning.
• Uses :
• End runner mill provides moderately fine
powder and operates successfully with fibrous
materials, bark, woods fruits, leaves, etc.
• Wet grinding with very viscous material such
as ointments and paste is also possible.
Edge runner mill
• Principle: shear and crushing
• Construction :
• Edge runner mill, also known as Chilean mill or Roller stone
mill consists of one or two heavy steel or granite rollers
mounted on a horizontal shaft and turned round a central
vertical shaft on a bed of steel or granite. The stones may vary
from 0.5 to 2.5 m in diameter, the larger size weighing up to
about 6 tons.
• The material to be ground is kept in the path of the runner by
scrapers. The reduction is partly due to crushing: by the
weight of the stones, but more to friction between the
surfaces of contact between the runners and the bed stone.
• Uses :, particularly for reducing extremely
tough and fibrous materials – roots and
barks to the form of powder.