UNIT-1
Size Reduction
Size Reduction also called as comminution or diminution or
pulverisation
Size reduction is achieved by the Precipitation method or
Mechanical process
Introduction
Advantages:
Content uniformity
Uniform flow
Effective extraction of drugs:
Mod. Coarse – Tincture: Coarse powder without
fine - percolation
Effective drying
Improved physical stability – Suspension &
emulsion
Improved dissolution rate
Introduction
Disadvantages:
Drug degradation: heat during milling, increased
Surface area.
Poor mixing – aggregation, adsorption of air
Contamination – wear off
Mechanism
Flaws in the particle (Impact) Crack (Further
impact) Smaller particle & Additional surface
Unmilled particle (Attrition) Edge break
small particles
Mode of Stress applied in size reduction
1. Cutting: The material is cut by sharp blades. Ex: Cutter Mill
2. Compression: The material is crushed between rollers. Ex:
Roller Mill
3. Impact: When a stationary material strikes the rotating
Hammers(Hammer Mill) or moving particles strike stationary
surfaces (Fluid energy Mill)
4. Attrition: This process involves breaking down of the
material by rubbing action between two surfaces. Ex: Fluid
energy Mill
Factors Affecting Size Reduction
Hardness Purityrequired
Toughness Ratio of feed size to
Abrasiveness product size
Stickiness Bulk density
Softening temperature
Material structure
Moisture content
Physiological effect
Factors Affecting Size Reduction
Hardness
It is a surface property of the material.
It is frequently confused with a property named strength.
Thus, it is possible for a material to be very hard, but if it is
brittle, then size reduction may present no special
problems.
An arbitrary scale of hardness has been devised known as
Moh’s Scale;
Moh's Scale = 1 is for graphite
Moh's Scale < 3 is for soft material
Moh's Scale > 7 is for hard
Scale = 10 is for diamond
The harder the material the more difficult it is to
Factors Affecting Size Reduction
Material structure:
Some substances are homogeneous in character.
Mineral substances may have lines of weakness
along which the materials split to form flake-like
particles.
Vegetable drugs have a cellular structure often
leading to long fibrous particles.
Factors Affecting Size Reduction
Abrasiveness:
Abrasiveness is a property of hard materials
(particularly those of mineral origin).
It may limit the type of machinery that can be
used.
During the grinding of some very abrasive
substances the final powder may be contaminated
with more than 0.1 percent of metal worn from
the grinding mill.
Factors Affecting Size Reduction
Softening temperature:
During the size reduction process, heat is
generated which may cause some substances to
soften, and the temperature at which this occurs
can be important.
Waxy substances, such as stearic acid, or drugs
containing oils or fats are examples that may be
affected.
Some methods can be used to overcome this like
the mill, either by a water jacket or by passing a
Factors Affecting Size Reduction
Friability:
The friability of the material is its tendency to
fracture during normal handling.
In general, a crystalline material will break along
well-defined planes and the power required for
crushing will increase as the particle size is
reduced.
Stickiness:
A sticky material will tend to clog the grinding
equipment and it should therefore be ground in a
Factors Affecting Size Reduction
Soapiness:
In general, this is a measure of the coefficient of
friction of the surface of the material. If the
coefficient of friction is low, the crushing may be
more difficult.
Explosive:
Such materials must be ground wet or in the
presence of an inert atmosphere.
Materials yielding dusts that are harmful to the
health:
Such material must be ground under conditions
CLASSIFICATION OF SIZE REDUCTION
EQUIPMENT
A. Crushers:
Edge runner mill, end runner mill
B. Grinders:
(1) Impact mill EX: Hammer mill.
(2) Rolling compression: EX: roller mill
(3) Attrition mill EX: attrition mill.
(4) Tumbling mill EX: ball mill.
C. Ultrafine grinder EX: fluid energy mill
D Cutting machine EX: cutter mill.
HAMMER MILL
Principle:
Impact between rapidly moving hammers
mounted on a rotor and the powder material.
Construction:
Horizontal or vertical shaft type
Hammers – hardened steel, stainless steel
Impact surface – extremely abrasive resistance
material (haystellite, carballoy)
HAMMER MILL
Bar shaped hammer – tablet
granulation
Hammer blades – flat edge /
sharp edge / both on each side
Rigid or swing-type
Swing type – increasing
clearance between hammers &
screen
Chamber containing grid or
removable screen perorated
holes or slotted type
Working:
Continuous motion – 8000 -
15000 rpm
HAMMER MILL
Rotating hammers beat material to smaller
particles
Pass through screen tangential exit size smaller
than aperture
Screens – interchangeable –
grades of fineness
Fineness regulated
Rotor speed
Feed rate
Clearance b/w hammers & grinding plate
No. & types of hammer
HAMMER MILL
Uses:
Particle size – 10 - 400 mm
Non-abrasive to moderately abrasive, brittle
material
Dry material, wet filter press cakes, ointment,
slurries
Brittle material – blunt hammer
Fibrous material – with cutting-edge
HAMMER MILL
Advantages:
Easy to install, dismantle & clean up
Minimal scale up problem
Occupies small space
Versatile: speed & screen can be changed rapidly
Operated in a closed environment – dust reduced,
explosion hazards prevented
Disadvantages:
Screens get clogged
Heat build up – product degradation
Wearing of mill & screen with abrasive material
Not employed for sticky, fibrous & hard materials
BALL MILL/ PEBBLE MILL/ TUMBLING MILL
Principle:
Impact between rapidly moving balls and the powder
material enclosed in hollow cylinder
At low speed – balls roll over each other attrition
predominates
Impact or attrition or both
Construction:
Hollow cylinder mounted on a metallic frame
rotated on its longitudinal axis
Length is slightly greater than diameter
Made of metal lined with chrome / rubber /
BALL MILL
Ball occupy 30 - 50% of mill volume
Ball size depends upon feed size & mill diameter
Balls: steel, iron, stoneware
Working:
Drug in cylinder (60% of volume) + Balls – rotate
on longitudinal axis
At low speed balls roll over each other
attrition predominates
Small balls greater surface
Attrition mode wet grinding
BALL MILL
At optimum(corrct) speed centrifugal force
balls are picked up by the mill wall carried near
to the top break contact fall to the bottom
Repetition of the processes
Impact mode more effective size reduction
At higher speeds centrifugal force balls are
thrown out to the wall no grinding
Compression by the ball with
wall not sufficient for effective
comminution.
BALL MILL
Uses:
Fine grinding – 100 - 5 mm or less
Hard & abrasive material
Ball mill at low speed – dyes, pigments &
insecticides
Advantages:
Produce very fine powder
Useful for batch operation, can be made
continuous operation
Suitable for both wet & dry grinding processes
BALL MILL
Operation can accomplished in inert atmosphere
oxygen sensitive substance
For sticky material
Installation, operation & labour costs low
Disadvantages:
Very noisy machine
Wear & tear contamination
Slow process
Not employed for soft, tacky, fibrous materials
FLUID ENERGY MILL / JET MILL /
MICRONIZERS / ULTRAFINE GRINDERS
Principle:
Impact and attrition
Feedstock is
suspended within a
high velocity of air
stream
High velocity
collision b/w
FLUID ENERGY MILL / JET MILL /
MICRONIZERS / ULTRAFINE GRINDERS
Construction:
Elliptical pipe height:
~ 2m; diameter: 20 - 200
mm
Mill surface soft
stainless steel / tough
ceramics
Contact surface with
linings removed or
replaced after excessive
FLUID ENERGY MILL
Grinding nozzle: 2 - 6 no. placed tangentially or
opposite to the initial flow path
Compressed air: 600 kilopascal to 1.0 megapascal
Inert gas: minimize or eliminate oxidation
Working:
Powder through inlet of venturi
Air through grinding nozzle transport powder in
the elliptical or circular track
Turbulent air stream suspended particles collides
& break
Impact & attrition forces
Small particles carried to outlet removed by
FLUID ENERGY MILL
Coarser particle recirculation due to own weight
Recirculated particles collision with new incoming
feed stock particles
Remain in the mill until size is reduced sufficiently
Particles entrapped by drag of gas leaves mill
cyclone separator / bag collector size separation
Uses:
Size reduction of antibiotics, vitamins
Preferred one in case of enhanced absorption/
bioavailability
FLUID ENERGY MILL
Advantages:
No moving parts no heat heat labile
substances : sulphonamides, antibiotics, vitamins;
suspension of gas under pressure cooling effect
Rapid & efficient method: 30 min. or less
No wear no contamination
Disadvantages:
Not suitable for soft, tacky & fibrous materials
Equipment is expensive
EDGE RUNNER MILL
Principle:
Crushing (compression) due to heavy weight of
the stones
Shearing force also involved during movement of
stones
Construction:
Two heavy rollers weighs several tons
Rollers move on bed : stones or granite
Rollers have central shaft & revolves on its axis
Roller are mounted on horizontal shaft & move
EDGE RUNNER MILL
Working:
Material placed on bed
Scrapper keep the material in the
path of the stone wheel
The stones revolves on its axis &
travel around shallow stone bed
Outer part of wheel travel a greater distance than
inner wheel size reduction is achieved by shearing
& crushing
Ground for a definite period collected sieve
Batch process
EDGE RUNNER MILL
Uses:
Tough material to fineDisadvantages:
powder Requires more space
For plant based Contamination of the
products product
Advantages: Time consuming
Does not require process
attention Not for sticky materials
Energy consumption is
END RUNNER MILL
Principle:
Crushing (compression) due to heavy weight of
the steel pestle
Shearing force also involved during movement of
mortar and pestle
Construction:
Mechanical mortar & pestle
Steel mortar fixed to a flanged plate
Underneath the flanged plate, a bevelled cog
fitting attached to a horizontal shaft bearing a
END RUNNER MILL
Pestle dumb-bell shaped flat bottom
Carries a hinged arm raised from the mortar
facilitate emptying & cleaning
The narrow central portion of pestle is longer
than the band of the arm around it pestle
can rise & fall over the material.
END RUNNER MILL
Working:
Material placed in mortar
Scrapper keep the material in the path of the
pestle
The mortar revolves at high speed
The pestle is placed in mortar
The revolving mortar cause the pestle to revolve
size reduction is achieved by shearing & crushing
collected sieved
END RUNNER MILL
Uses:
Suitable for fine powder
Disadvantages:
Not suitable for unbroken or slightly broken
materials
Theories
Griffith theory
All Solids contain flaws and microscopic crack
A Flaws is a structural weakness that may develop into
a crack under the strain
The weakest flaw in a particle determines its fracture
strength. It controls no. of particles produced by
fracture
Particles with the weakest flaw fracture most easily and
produce the largest possible pieces
The next step is another weakest flaw fractured, this
continues until all flaws fractured
Theories
Griffith
theory:
The amount of force to be applied depends on the
crack length and focus of strength at the atomic
bond of the crack apex. 𝒀𝜺
𝑻=
𝒄
T=tensile strength
Y=Young’s modulus
ε = surface energy
C= critical crack path required for fractured
A linear relationship b/w the sq. of tensile strength
of mineral and critical height for drop weight
THEORIES OF SIZE REDUCTION / MILLING
A number of theories have been proposed to establish a
relationship between energy input and the degree of size
reduction produced.
•Rittinger’s theory
•Bond’s theory
•Kick’s theory
Rittingers Theory
According to this law, the energy required for size reduction of unit mass is
directly proportional to the new surface area produced. (brittle)
Mathematically, Different materials have different Rittinger’s numbers and
can be obtained by drop weight test.
E=KR(Sn – Si )
KR = Rittinger constant
Sn = New specific surface area
Si = Initial specific surface area
E = Amount of energy
Kicks Theory
•Kick’s law: The energy used in deforming or fracturing a set of particles of
equivalent shape is proportional to the ratio of the change in size.
𝒅𝒊
• 𝐸=𝐾𝐾 𝑙𝑛
𝒅𝒏
• KK= Kick’s constant,
•di (m) = Diameter of the particle in the initial stage
•dn (m) = Diameter of the new particle
• di/dn = Ratio of the change in size (size reduction ratio)
di/dn is used to evaluate the relative performance of different types of
equipment.
E=ENERGY
Limitation
Both Kick’s law and Rittinger’s law have been shown to apply over limited
ranges of particle size, provided KR and KK are determined experimentally
by testing in machine of type to be used and material to be crushed. Thus,
they have limited utility.
Bonds Theory
Bond’s law: The Energy used in crack propagation (size reduction) is
proportional to the length of the new crack produced.
𝐸 = 2 KB (1/ 𝒅𝒏 - 1/ 𝒅𝒊 )
E([Link]-1) = the energy required per mass of feed
KB= Bonds Work Index (work required to reduce a unit weight)
di (m) =Initial diameter of the particle
dn (m) = New diameter of the particle
Bonds Work Index (KB):
The work required to reduce a unit weight from the
theoretical infinite size to 80% passing 100 µm.
This law is useful for rough mill sizing
The work index is useful for comparing the efficiency of
milling operations