Size reduction

Objectives

1. To define size reduction

2. To discuss the advantages and disadvantages of size reduction
3. To explain the influence of material properties on size reduction
4. To discuss methods of size reduction

Size reduction is a process of reducing large solid unit masses of particles to

small unit masses of coarse particles or fine particles.

Size reduction is also termed as comminution, diminution or

pulverization. It can be achieved by two methods i.e. precipitation or
mechanical methods.

Advantages of size reduction

Content uniformity: better content uniformity is achieved by size reduction.

Uniform flow: smaller particle size and controlled size distribution promote
the flow of the powder into dies during compression of tablets.

Effective extraction of drugs: small particles allow penetration of menstruum

or solvent into inter-particle space.

Effective drying: drying of a granular mass can be rapid and effective, if the
size of granules is small and uniform.

Improved physical stability: in cases of suspension and emulsion, the rate of

sedimentation decreases to a large extent if particle size is small.

Improved dissolution rate: size reduction increases surface area, which

facilitates intimate contact of solid particles and gastric or intestinal juices.

Improved rate of absorption: the smaller the particle size, the faster the rate
of absortion. e.g. griseofulvin should have a surface of not less than 1300
and not more than 1700 per Kg.

Disadvantages of size reduction

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Drug degradation: drug decomposition is possible due to the heat generated
during milling. Thermolabile substances are most affected. Cooling support
systems are provided to decrease the heat in milling equipment.

Poor mixing: normally, very small particles contain strong cohesive forces
hence aggregation of particles is possible.

Contamination: during milling, the grinding surfaces wear off, the particles of
which become present as impurities in the powder.

Influence of material properties on size reduction

Cracking and propagation

Size reduction is carried out by a process of crack propagation whereby

localized stresses produce strain in the particles which are large enough to
cause bond rapture and thus propagate the crack. In general, cracks are
propagated through regions of a material that posses the most flaws or
discontinuities and are related to strain energy in specific regions according
to Griffin’s theory of crack propagation. The stress in a material is
concentrated at the tip of a crack and the stress multiplier can be calculated
from an equation developed by Inglis;

δk = 1+ 2(L/2r)

where δk is the multiplier of the mean stress in a material around a crack. L

is the length of the crack and r is the radius of curvature of the crack tip. The
stress concentration decreases towards the mean stress according to the
distance from the crack tip. The crack tip propagates at a velocity of
approaching 40% of the speed of sound in the solid. The excess energy from
strain relaxation is dissipated through the material and concentrates at other
discontinuities.

Surface hardness

Size reduction can be influenced by surface hardness. The hardness is

measured in a scale of mohs. The hardest material, diamond has a value
more than 7 and the softest is talc with a value less than3. Soft materials

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absorb large amounts of energy through elastic and plastic deformation and
hence are difficult to crack.

Particles with moisture content below 5% can undergo dry grinding, above
50% moisture content, they can undergo wet grinding.

Energy requirements of size reduction process

Only small amounts of energy put in communition actually effects the
process. As little as 2% of the total energy is used. Most energy is used in
many ways including:

 Elastic deformation of particles

 Plastic deformation of particles without fracture

 Deformation to initiate cracks that cause fracture

 Deformation of metal machine parts

 Interparticulate friction

 Particle- machine wall friction

 Heat

 Sound

 Vibration

Energy in-put in relation to size reduction can be given by the hypotheses

below:

Rittinger’s hypothesis

Is usually interpreted according to the energy E, which is proportional to the

new surface area produced sn

E= KR (Sn-Si)

Where Si is the initial surface area, K R is Rittinger’s constant of energy per

unit area.

Kick’s theory
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States that the energy used in deforming or fracturing a set of particles of
equivalent shape is proportional to the ratio of change in size;

E = Kk log di/dn

Where Kk is Kick’s constant of energy par unit mass, d i is the initial particle
diameter, dn the new particle diameter.

Bond theory

States that energy used in crack propagation is proportional to new crack

length produced, which is often related to the change in the particle
dimensions according to the following equation;

E = 2KB (1/dn-1/di)

KB is the bond’s work index and represents the variation in materials and
size reduction methods.

Walker proposed a generalized differential form of the energy-size

relationship which is a relationship between Kick and Rittinger’s equation:

∂E = KW ∂d/dn

kw is walker’s constant, d is the size function that can be characterized by

integrated mean size or by weight function. When designing the milling
process, it is advisable to select the most appropriate hypothesis.

Methods of size reduction

The extent of size reduction is determined by the milling time.

The common modes of size reduction include:

1. Cutting by use of a sharp blade(s) e.g. cutter mill

2. Compression where material is crushed between rollers by

application of pressure e.g. roller mills

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 3. Impact which involves the operation of hammers or bars at high
speed. e.g. fluid energy mill.

4. Attrition involves breaking down of the material by rubbing action

between two surfaces. E.g. fluid energy mill.

Classification of size reduction equipment

1. Crushers e.g. edge runner mills, end runner mills

2. Grinders a) impact mills e.g. hammer mills

b) Rolling compression e.g. roller mills

c) Attrition mills e.g. attrition mills

d) Tumbling mills e.g. ball mills

3. Ultra fine grinders e.g. fluid energy mill

4. Cutting machine, e.g. cutter mill

General parts of size reduction equipment

The equipments consist of three major parts:

1. A structure for feeding material into the mill; the hopper

2. The milling chamber which consists of a rotor and stator

3. A discharge chute or receiver where milled product is collected.

4. Other accessories include the sieves/ screen to classify materials by

size, cyclone separator or centrifuge equipment for size separation,
dust collectors to collect fine dust

Cutting method

Principle: size reduction involves successive cutting or shearing the feed

material with the help of a sharp knife. The high shear rates present in cutter
mills are useful in producing a coarse degree of size reduction of dried
granulation prior to tablet.

Diagram:

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Variants: double-runner disc mill: consists of two vertical mills, each rotating
in opposite direction. Single-runner disc mills consist of one disc mill rotating
while the other is stationary.

Impact methods

Size reduction is carried out using hammer mill. The mill consists of four or
more hammers enclosed in a rigid metal case. During milling, the hammers
swing out radially from the rotating central shaft. As size reduction
continues, the inertia of particles hitting the hammers reduces markedly and
subsequent fractures of particles are less probable. Hammer mills hence
produce particles of varied size ranges. Particles produced can be finer than
mesh aperture since they pass tangentially.

An alternative to the hammer mill is the vibration mills. The mill is filled to
80% capacity with steel or porcelain balls and milling occurs by vibration.
Commuted materials fall through a screen placed below.

Diagram :

Attrition mills

Roller mills use the principle of attrition to produce size reduction by

attrition. Two or three porcelain or metal rolls are mounted horizontally with
an adjustable gap approximately 20ᶙm. The rollers rotate at different speeds
so that the material is sheared as it passes through the gap. The ground
material is removed by a scrap.

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Combined impact and attrition methods

A ball mill combines both methods. It consists of a hollow cylinder mounted

such that it can be rotated on its horizontal longitudinal axis. The balls
occupy 30-40% of the total volume, ball size is dependent on feed and mill
size.

The amount of materials in the mill is important, too much produces

cushioning effect and too little causes inefficiency. The speed of rotation of
the mill is of greatest important, too fast speed causes balls to be aligned on
the walls while too slow speed doesn’t cause change in size reduction.
Optimum speed is recommended.

Diagram :

Alternative techniques

Fluid energy milling is a form of size reduction method that acts by particle
impaction and attrition. This type of mill or micronizer consists of a hollow
toroid which has a diameter of 20-200mm. A fluid, usually air is injected at a
high pressure-pressure jet through nozzles at the bottom of the loop. The
high velocity of air causes a zone of turbulence into which solid particles are
fed. The high kinetic energy of the air causes particles to impact with others
with sufficient momentum for fracture to occur. A particle size classifier is
incorporated so that larger particles are retained in the toroid long enough
for reduction to occur.

Factors determining choice of reduction method

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1. The desired use of the powder

2. The particle properties of the powder e.g. hardness, toughness, sticky,

friable e.t.c.