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PARTICLE SIZING - MILLING

o The pharmaceutical importance of particle sizing

o Milling Theories
o Differentiate between the various methods used in milling

 particle size reduction

During raw material manufacturing, solid produced = larger size than required

The method used for size reduction (COMMINUTION) affects:

- mean particle size
- distribution

Efficient size reduction requires: Stoke’s Law

- machinery properties
- mechanisms

Size reduction = more efficient processes e.g. mixing/suspension production

Smaller size = material floating in the system for longer because sedimentation rate =
lower = the stability of suspension is higher

Material of different size mixed together causes segregation which means separation
according to size

 crack propagation

Takes place during size reduction

High localised stress = strain in particles  causes bond rupture and propagation of crack

Mean stress around crack = crack multiplier

For material to propagate crack = brittle

Plastic material = relaxation without propagation as atoms flip over one another so they
won’t break.

Elastic = go back to shape

 Surface hardness
- Mohs’s scale :
Talc (used as lubricant) = 3
Diamond = 7
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Important because when you decide what equipment you want to use to break down
pharmaceutical material, like stainless steel, to withstand the reduction process so it
will last longer

- Brinell :
Quantitate measurement
Known constant load applied on spherical indenter  in contact with testing material
Permanent deformation formed is used to calculate the material hardness
used to work out how hard the material is

- Very hard material and elastic materials are difficult to comminute

- Lowering the temperature for elastic mats. Below Tg (glass transition temp) to enable
size reduction and material will behave like glass and shatter with added pressure

 Energy Requirement

- Particle size reduction process requires energy

- 2% of total energy applied
- Remaining used in :
elastic, plastic deformation
interparticulate friction
heat
sound
vibration

HOW TO CALCULATE HOW MUCH ENERGY IS SUPPLIED

Rittinger’s hypothesis
- Related energy used for size reduction to surface area
- Energy is directly proportional to change in surface area

Kick’s theory
- Related the energy used for size reduction to ratio of change on size
- Energy directly proportional to log(initial diameter/new diameter)

 Cutting methods

- Cutter mill
Series of knives attached to rotor and move against series of stationary knives
attached to the casing
Escape through screen made up of stainless steel
Size reduction = 100 – 50,000 um

 impact methods

- Hammer mill
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Made up of 4 or more hammers attached to central shaft

Enclosed by rigid metal case
Hammers move radially
Angular velocity = strain rate of 80/s = high enough for particles to undergo brittle
fracture
Size reduction = 50 – 5,000 um

- Vibrational mill
80% of mill is filled with porcelain or stainless steel balls vibrate via springs
Size reduction = 1-1000um

Factors that affect particle size in vibrational mill

@ size of balls ,, bigger balls more impact force so smaller size
@ magnitude of vibration

 attrition methods
- Roller mill
Made up of 2/3 porcelain/metal rollers mounted horizontally and separated by a gap
(20um)
When particle passes into gap, shearing takes place
Size reduction (1-200um)

 combined impact and attrition

- Ball mill
Conssits of hollow cylinder rotates at high speed
30-50% of the cylinder is filled with balls

Too high speed = balls thorwn out to the mill wall by centrifugal force and no size
reduction occurs

Too low speed = very little movement of balls and minimal size reduction

Optimum 2/3 of critical angular velocity = cascading action  balls lifted on rising
side of drum until dynamic angle of repose is exceeded then balls fall to the base of
the drum

Size reduction (1-200um)

 fluid energy mill

- Hollow toroids of diameter of 20-200mm

- Air injected as high pressure jet through nozzles resulting in forming zones of
turbulence
- Coarse particles are retained in the toroid by means of particle size classifier until
sufficiently fine

 compression methods

- Runner mill
Size reduction (20-10000um)
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- Roller mill
Two cylindrical roller rotate
One of the rollers is driven directly while introfucing the particles between the 2
rollers drives the rotation of the second rollers friction

Size reduction (500-100,000um)