SIZE REDUCTION

Large size particle

Small size particle

Unit operation process .

DEFINITION
Process of reducing large solid unit masses in to small unit masses

(Coarse particles or fine particles )

Normally pharmaceutical powders – polydisperse (different particle size)

Difficulties in the production of dosage forms

This problem can be overcome by using monosize powder particles .

( size reduction and size separation process used )
 Size reduction is also known as comminution or diminution or
pulverisation or milling or trituration or grinding or levigation

size reduction can be achieved by two methods

1. Precipitation method ( drug + solvent 1+ solvent 2 = finely precipitated)

This method suitable for API production

2. Mechanical process
( mechanical forces using grinding equipment's)

Eg . Ball mill
Cutter mill
Roller mill
Hammer mill
Types of Milling - Dry milling( Used in Tablet , capsule production)
Wet milling ( Used in suspension , emulsion production)

This method most commonly used in API and dosage forms manufacturing
Advantage of size reduction

 To achieve effective mixing of different ingredients if the particles are uniform and
small

 Enhance powder flow from hopper in to die cavities of tablet compression machine

 Effective extraction of drugs ( herbal extracts – galenical preparation- percolation,

maceration)

 To achieve Effective drying – if granules size are small and uniform.

 To Improves physical stability of suspension and emulsion ( small particle –sedimentation

decrease)
 To enhance drug solubility , drug dissolution.

 To enhance the drug absorption ( Dry powder inhaler (dpi) formulation –Asthma)
 DISADVANTAGE

 Drug degradation / decomposition of drugs (due to heat produced in milling

process) .

eg . Thermolabile drugs , waxy materials mostly affected )- over come by cooling

support system

 Aggregation of powder – if too fine powders - poor mixing

 Metal contamination –Grinding surfaces wear off

Mechanisms of size reduction

Particles - crystalline or
amorphous will have flaws .

Sufficient stresses are applied

on weak flaws in to cracks ,
cleavage in to smaller particles.
 TYPES OF STRESS APPLIED ON SIZE REDUCTION

Cutting –materials cut by means of sharp blades eg. Cutter mill

Compression – materials crushed between rollers by applying pressure. Eg roller mill

Impact – lump of materials are size reduced by rotating hammers eg. Hammer mill

Impact also occurs when moving particles strike against stationary surface
( at high speed particle -particle collide each other to produce small particles) eg. Fluid
energy mill

Attrition-breaking the materials by rubbing action between two surface

Eg. Fluid energy mill

Classification of size reduction equipment's

Crusher
Edge runner mill , end runner mill
Grinders
Impact mill eg. Hammer mill
Rolling- compression mill eg . Roller mill
Attrition mill eg . Fluid energy mill
Tumbling mill eg. Ball mill
Ultrafine grinder eg. Fluid energy mill
Cutting machines eg. Cutter mill
SELECTION OF MILL

Depends on physical properties of raw materials (feed of equipment)

 Hard materials
 Fibrous materials( ginger , rauwolfia)
 Wax and resins (elastic materials)
 Hygroscopic materials
 Low melting points materials
 Thermolabile materials
 Moisture content – below 5% suitable for dry milling 5-50 %
suitable for wet milling
 RITTINGER'S THEORY

states that the energy required for size reduction is directly

proportional to the new surface area created.

Smaller Particles = large Surface Area

it is typically used for fine grinding.

 BOND'S THEORY

states that the energy required to reduce the size of particles

is proportional to the square root of the of the particles.

Applicable for intermediate size reduction

process,when particles are neither too large nor
extremely fine.
 KICK'S
THEORY
the energy required for size reduction is inversely
proportional to the particle size.
HAMMER MILL /CRUSHER
Principle :

Impact mechanism
Impact between rapidly moving hammers mounted on a rotor and feed the
material.
Construction:
 Hopper (Feed inlet )
 Milling chamber
 Hammer mill two type vertical or horizontal type
 Hammers made of stainless steel(carbaloy)
 Hammers several shapes (stirrup and bar)
 Hammer bar with sharp edges blade
 Screen/sieves
 Discharge chute /feed outlet
Working :

• Hammers are allowed to be in continuous motion (8000-15000 rpm)

• The feed materials is placed in to the hopper which flows vertically

down and then horizontally while hammers are continuous motion.

• Rotating hammers beat the materials to yield smaller particles .Then

these particles pass through screen .

• Screen are interchangeable

Uses:
fine to moderate grinding of powders may be obtained.

Expected particle size may vary from 10 to 400 µm

To mill dry materials,ointment

Brittle materials can be used as feed stock

Disadvantage : heat build-up, not suitable fibrous ,hard materials .

BALL MILL OR PEBBLE MILL OR TUMBLING MILLS

Principle :

Impact and attrition- Rubbing action

(predominant )

Impact between rapidly moving balls and feed

materials in a hollow cylinder.
Construction :
Hollow cylinder mounted on metallic frame rotated on its
longitudinal axis.

Length of the cylinder(lined with chrome) is greater than

diameter.
• Cylinder contains balls that occupy 30-50% of the mill volume.
• Balls made of steel , iron.( acts as grinding medium )

Working :
Feed the cylinder with number of balls.
At low speed the balls roll each other and attrition will be predominant .

At high speed the balls are thrown out to the walls by centrifugal
force .grinding will not occur.

At correct speed the centrifugal force just occurs as a result the balls are
picked up by wall and carried nearly top and fall to the bottom (impact )
FLUID ENERGY MILL OR JET MILL OR MICRONIZER OR ULTRASONIC
GRINDERS
Principle : impact and attrition mechanism

Milling takes place , because of high velocity air stream

causes collisions between the suspended particles.

Construction :
 Elliptical pipe – 2 meter height ,20-200 mm diameter.
 Grinding nozzle (fluid nozzle) may be placed
tangential and or opposed to air flow.
 Compressed air – 600 kilopascals to 1 megapascal
 Inert gas – prevent oxidation
 Venturi feeder –provide path of air flow.
 Outlet with bag filter / cyclone separator –to escape
of air.
Working :
Powder is introduced through inlet of venturi.
• Air entering through grinding nozzle transport the powder in the elliptical tank .

• In the turbulent air stream of air , the suspended particles collide with each other and
break.

• The resultant small particles are carried to outlet and removed by cyclone separator .

• Coarse particle undergo recirculation and collide again with new incoming feed stock
particles. Later leaves via screen.

Advantage : Antibiotics , vitamins size reduction .

Disadvantage : Not suitable for tacky , fibrous materials .

 EDGE RUNNER MILL
Principle : size reduction done by compression due to
heavy weight stones. Shearing force is also involved during
the movement of stones.

Construction : consist of two heavy rollers

• Rollers move on bed ( stone or granite )
• Each roller has central shaft and move around the bed.

Working :
 Feed stock placed on the bed.
 Help of scrapper feed are kept in the path stone wheel.
 Powder is collected and passed through to get desirable
size.
 END RUNNER MILL
Principle :
 Size reduction can be done by compression ( crushing) using heavy
weight pestle .
 Shearing stress is also involved during the movement of mortar and
pestle.

Construction : mechanical mortar pestle

 Pestle –dumb bell shape .
 Th bottom of pestle is flat rather than round.
 Pestle can be raised from mortar for cleaning and fall over the
material.
Working :
 Feed stock placed in the mortar.
 Scrapper puts the material in the path of pestle.
 Mortar revolves at high speed
 Pestle placed in the mortar . Rotating mortar causes the pestle to
revolve .
 Powdered materials passed through a sieve to get desirable size.

Use: suitable for fine grinding