Milling

• Mechanical process to reduce the size of particles.

• Crushing, disintegration, pulverization, dispersion and grinding
• Equipment classified as course, intermediate and fine. (Mesh size is no. of opening per
linear inch of surface). Course > 20 mesh, intermediate 20-200 and fine < 200mesh size.
Applications
• Specific surface (surface area per unit weight) increases with size reduction. Increases
the therapeutic efficiency of low soluble compounds.
• Control of particle size and specific surface affects the duration of adequate serum
concentration, rheology and product syringiability of a suspension of Penicillin G.
• Increased antiseptic action of calomel.
• Reduction in extraction time and dissolution time.
• Mixing or blending is easier with ingredients of same size.
• Solid pharmaceuticals that are artificially coloured are often milled to distribute the colouring agent and to
ensure that the mixture is not mottled and is uniform batch to batch.
• Lubricants used in compressed tablets and capsules formation needs to be fine in size.
Size distribution and management
• Normally size is irregular ranging from large to small.
• Statistical methods are there to express the size of an irregular particle in terms of a single dimension
referred to as its diameter.
• An irregular particle considered as an equivalent sphere if have the same surface area or volume with the
diameter d.
• The volume of a particle is determined by displacement in a liquid and equated to the volume of a
hypothetical sphere possessing as an equivalent diameter.
• The arithmetic and geometric mean and the median diameter have no physical significance,
meaning choice of diameter depends on its relevance to some significant physical property.
• The packing and flow of a powder or granulation depends on its volume, thus if packing is the
prime consideration, the size should be expressed as a mean volume diameter.

• Dissolution and adsorption process are a function of the surface area of the particle and with
these processes, the particle size should be expressed as mean surface diameter.
• As sedimentation is important property of suspensions, the size of the suspended particles should
be expressed as Stokes diameter.
• The Stokes diameter is the diameter of a sphere that requires the same time to settle between
fixed points in the liquid as does the irregular particle. (sedimentation)
Microscopy:
• Size analysis by light microscopy is carried out on the two-dimensional images of
particles which are generally assumed to be randomly oriented in three dimensions except
for dendrites, fibres or flakes. Under such conditions, size analysis is carried out accepting
that they are viewed in their most stable orientation.
• SEM and TEM analysis is done when a three dimensional particle image is required; in
addition, the very much greater depth of field of an SEM compared to a light microscope
may also be beneficial. Both allow the lower particle-sizing limit to be greatly extended
over that possible with a light microscope.
Sieving: Its is most widely used method, inexpensive, simple and rapid. Drawback is the
lower limit being 50microns, with micromesh size, it will be 10 microns.
• In US two standards of sieves are being used: Tyler Standard scale, the ratio of the width
of the opening in successive sieve is √2. This is based on the size of opening in wire
cloth having 200 opening per linear inch i.e. 200 mesh size. The National Bereau of
Standards uses the ratio of √2, but it is based on the opening of 1mm (18 mesh).
• Procedure: The mechanical shaking of a sample through a series of successively smaller
sieves, and the weighing of the portion of the sample retained on each sieve.
• Vibratory motion is the most efficient followed successively by side tap motion, bottom
tap motion, rotary motion. Time also plays an important role. The load or the thickness of
powder per unit area of sieve, influences the time of sieving, which is roughly
proportional. Therefore, in size analysis by means of sieving, the type of motion, time and
load should be standardized.
• If the weight distribution obtained by sieving follows a logarithm-probability distribution,
the Hatch-Choate equations permit conversions of the weight to a number distribution.
Comminution:The process of reducing the particle size of a substance to a finer state or powder is
known as comminution.
It is done with the help of mortar and pestle or mills.
Different mills used for the reduction of particle size are hammer mill, ball mill, colloid mill, fluid
energy mill, etc.
Objectives/Advantages of Size Reduction:
1. To produce smaller particles.
2. To increase surface area.
3. To achieve proper mixing.
4. To improve handling of powders.
5. To prepare pharmaceutical dispersions.
6. To improve the flow of powder.
7. To improve physical stability.
8. To improve dissolution rate of powders.
9. To improve rate of absorption and to improve the extraction process.
• Most efficient mills utilize less than 1% of
energy input to fracture particles and create
new surfaces. The rest of the energy is
dissipated in elastic deformation of
unfractured particles, transport of material
within the milling chamber, friction
between particles, and mill heat, vibration
and noise, and inefficiency of transmission
and motor.
• The immediate objective of the milling is to
form the cracks that spread through the
deformed particles at the expense of strain
energy and produce fracture. The useful
work is directly proportional to the new
surface area.
• The expended energy can be calculated with the crack length and new surface area. Since the
crack length is proportional to the square root of the new surface area produced, the useful work
is inversely proportional to the square root of the difference of feed diameter and product
diameter. The energy Eˈ expended in producing new surface is :

Where D1 is the diameter of the material fed to the mill, D2 is the diameter of the product
discharged from the mill and E is the energy input.
• The efficiency of the milling process is influenced by the nature of the force as well as by its
magnitude. The rate of application of force affects comminution, as there is a time lag between
the attainment of maximum force and fracture.
• Often, materials respond as brittle materials to fast impact and act as plastic materials to a slow
force.
• The greater the rate at which the force is applied, the less effectively the energy is utilized, and
the higher is the proportion of fine material produced.
• As the rate of milling is increased, more energy is expended. To produce a new surfaces in
milliseconds may require three to four times energy as the production of the same new surface
area in seconds.
Factors affecting size reduction
Hardness: Hardness is the resistance of a material to deformation. It is measured using Moh’s scale
(1-10) from graphite to diamond.
Toughness: Toughness is the ability of a material to absorb energy and resist impact. Soft but tough
material is more difficult to reduce size than hard but brittle. e.g: toughness-rubber &
hardness-chalk
Abrasiveness: It is the property of hard materials especially minerals that causes scraping or
wearing of machine. Abrasive substance when reduced in size may contain 0.1% metal from
machine
Stickiness: It is the property of a material to stick to the machine parts during size reduction and
block the parts. Drying or addition of inert substance may help in sticky materials. e.g: gum, resins
Softening temperature: Temperature required to soften or melt materials is important in size
reduction. So, temperature should be kept low to avoid softening of materials and reduce their size.
e.g: waxy substance can melt at high temperature.
Moisture content: Moisture content of a material can affect its hardness, toughness or
stickiness. Generally materials should be dry and contain less than 5% moisture.
Bulk density: Bulk density of powder is the defined as the mass per unit volume.
Higher density means less volume occupied and more batch capacity.
Physiological effects: Some substances are very potent (podophyllum, hormones,
griseofulvin) and dust may effect person. So, such substances should be grinded on
closed mills.
Ratio of feed size to product size: The amount of material feed affects the product
size. So, size reduction may be done in several stages with different equipment. e.g:
coarse grinding followed by fine grinding.
• The resident time of milling is an important factor. When time is brief, the
material subjected to a relatively constant fracture- producing environment.
Changes in milling conditions that are insignificant for short milling periods may
be controlling factors in prolonged milling.
• As size reduction proceeds, the mean stress required to cause fracture increases
through the depletion of cracks, while the magnitude of available local stress
decreases. Because of diminishing local stress and increasing aggregation,
increase in energy expenditures are useless and size reduction reaches some
practical milling limit.
Principals of size reduction

• Cutting: The material is cut into small pieces by means of shape blade. e.g: cutter mill

• Compression: The material is crushed by the application of pressure. e.g: mortar and pestle, colloid mill

• Impact: The material is stationery and hit by a moving object at high speed or vice versa. e.g: hammer mill

• Attrition: The material is in motion with the surface and the pressure is applied to the material. e.g: roller mill,
fluid energy mill

Parts of mill: feed chute, grinding mechanism and a discharge unit. The principal operation depends on the direct
pressure, impact from a sharp blow, attrition or cutting. In most cases, it is combination of all these action.

Generally when the rate of feed is slow and discharge rate is fast, the amount of undersize or fines is minimum.
If the mill is choke fed at a faster rate and discharge rate is slow, this leads to greater reduction of particle size,
but the capacity of the mill is reduced and power consumption is increased. Choke fed is used when a small
amount of material is to be milled in one operation.

The feed rate should be equal to discharge rate, so that the milling parts can operate effectively.
• Mostly the gravitational force is sufficient to remove
the discharge but sometimes steam, air or inert gas
removes the product from the attrition, fluid-energy
or high speed hammer mill. For ultrafine grinding,
the force of gravity is replaced by fluid carrier. The
powder is removed from the fluid by cyclone
separators or bag filters.
• If the milling operation is carried out so that the
material is reduced to the desired size by passing it
once through the mill, the process is known as open
circuit milling. A closed circuit mill is one in which
the discharge from the milling chamber is passed
through a size separation device or classifier and the
oversize particles are returned to the grinding
chamber for further reduction of size. It is most
valuable in reduction to fine and ultrafine size.
Hammer mills crush materials into two (2) stages.
1. Size reduction which occurs by dynamic impact
2. Sizing which occurs by attrition and shear in the second zone where small clearance
exists between the hammer and the screen bar producing a particle range of 15-50 µm.
Pharmaceutical uses of Hammer Mill
1. It is used in pharmaceutical industries to process wet or dry granulations and disperse
powder mixtures.
2. It is used in milling pharmaceutical raw materials, herbal medicine, and sugar.
3. It is used in powdering of barks, leaves, and roots of medicinal plants.
4. It is applied in the milling of Active Pharmaceutical Ingredient (API), excipients, etc.
Hammer mill

https://www.youtube.com/watch?v=fSTvbE77ucE
Advantages:
1. It produces specified top size without the need for a closed-circuit crushing system.
2. It produces relatively numerous size distributions with a minimum of fines due to
self-classification.
3. It has a high reduction ratio and high capacity whether used for primary, secondary or
tertiary grinding.
4. Relatively reasonable energy requirements.
5. Brittle materials are best fractured by impact from blunt hammers.
6. It is capable of grinding many different types of materials
7. The machine is easy to install and operate and its operation is continuous.
8. It occupies small space
9. It is easy to maintain and clean.
10. It is inexpensive
Disadvantages of Hammer Mill
1. Not recommended for the fine grinding of very hard and abrasive material due to
excessive wear.
2. Not suitable for low-melting sticky or plastic-like material due to heat generation in the
mill head as a result of mill fouling.
3. The mill may be choked if the feed rate is not controlled, leading to damage.
4. Presence of foreign materials like stone or metals which finds its way into the material
due to inadequate garbling process
5. There is a possibility of clogging of the screen.
Ball Mill: Consists of horizontally rotating hollow vessels of cylindric shape with
length slightly greater than its diameter.
• Filled with balls of steel or pebble, which act as grinding medium.
• If rod or bars are used, its known as rod mill. Useful for sticky material.
• Tube mill is modified ball mill with length is four times more of diameter with
smaller balls. Fine grinding because of more resident time.
• Mostly ball mills are batch operated, however can be continuous with coarse
screen to protect balls.
• Communition is due to impact and attrition.
• https://www.youtube.com/watch?v=bljhXsH8-ME
• Critical speed: Speed of mill at which balls start centrifuge.

• The critical speed is

Where D is the diameter of the mill in feet.

• A larger mill reaches its critical speed at a slower revolution rate than a smaller mill.
• Generally operated at 60-85% of the critical speed. Though the output increases with
speed but for finer grinding, lower speed is better.
• The optimum speed is n = 57- 40 log D, where n is the speed in revolution per minute and
D is inside diameter in feet.
• Size of ball: small size gives slow but finer grinding (less void and high impact) though ineffective
in reducing large size feed.
• Optimum diameter: Dball2 = kD
• Ball charge: percentage of volume of the mill optimum range 30-50%
• Feed charge: material to void ratio (void space in the bulk volume of ball charge)
• Density of the balls: higher the density, better is the grinding. Stainless steel vs porcelain balls.
Less attrition and contamination.
• Dry vs wet grinding: Can be used for both. In dry, moisture should be less than 2%. With wet
milling, ball mill produces 200 mesh size particles from slurries containing 30-60% solids.
• Wet is better with respect to power consumption but speed should be low in wet.
• High viscosity restricts the motion of the grinding medium and the impact is reduced.
Sometimes wetting agent being added to nullify the electrostatic charge while grinding. This
also helps in size reduction and reduce aggregation.
Advantages of ball mill
1. It produces very fine powders.
2. It can grind different types of materials from wet to dry.
3. Tube mill can be used for continuous operation.
4. They are simple to operate and clean.
5. Ball mill is used in completely closed form so suitable for toxic materials.
Disadvantages of Ball Mills
1. Contamination of product may occur as a result of wear and tear which occurs
principally from the balls and partially from the casing.
2. High machine noise level especially if the hollow cylinder is made of metal, but
much less if rubber is used.
3. Relatively long milling time.
4. It is difficult to clean the machine after use.
Fluid energy mill: It is also known as jet mill, ultrafine
grinding mill or micronizer.
• It works on principle of impact and attrition. A fluid (usually
air or steam) is passed through the nozzle at high pressure
which will move the materials at high velocity with
turbulence.
• It consists of a loop of a 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 meters, a fluid, usually air, is injected
at high pressure through nozzles at the bottom of the loop,
giving rise to a high velocity circulation in a very turbulent
condition. Solids are introduced into the stream and, as a
result of the high degree of turbulence, impact and attritional
forces occur between the particles.
 • The large particles are carried by centrifugal force to the periphery, where they are further
exposed to attrition action.
• The fluid mill provides internal classification, which permits finer and lighter particles to
be discharged whereas heavier oversized particles will be remained under the effect of
centrifugal force till they reduce to small size.
• The feed to the mill needs to be pre-treated to reduce the particles size to the order of 100
mesh, enabling the process to yield a product as small as 5 micrometers or less.
• Advantages:
1. The particle size of the product is smaller than that produced by any other method of
size reduction.
2. Expansion of gases at the nozzles leads to cooling, counteracting the usual frictional
heat which can affect heat-sensitive materials.
3. Since the size reduction is by inter-particulate attrition there is little or no abrasion of
the mill and so virtually no contamination of the product.
4. For special cases with very sensitive materials it is possible to use inert gases.
5. Having a classifier as an integral part of the system permits close control of particle size
and of particle size distribution.
Cutting mill: Used for tough, fibrous materials and provide a successive cutting or shearing
action rather attrition or impact.
• The rotary knife cutter has horizontal rotor with two to 12 knives spaced uniformly from
200 to 900 rpm and a cylindric casing having several stationary knives. The bottom of the
mill holds screen that controls the size of the material discharged from the mill.
• Particles size are determined by a) Rotor size (b) The gap between the two sets of knives
(c) Screen size
• The feed size should be less than 1 inch thick and should not exceed the length of cutting knife.
• For size less than 20 mesh, a pneumatic product collecting system is required. The size limit is 80
mesh.
• Disc mill consists of two vertical discs; each may rotate in opposite direction (double runner disc
mill) or only one may rotate (single runner disc mill) with an adjustable clearances. The disc can
have cutting faces, teeth or convulsions.
Advantages of Cutter Mill
• 1. It is the best option of size reduction when impact, attrition, or compaction type milling is not
effective especially for tough, fibrous, or resilient materials.
• 2. It is easy to install, operate, and maintain.
• 3. The equipment is not expensive
Disadvantages of Cutter Mill
• 1. Cutter mill is not suitable for most pharmaceutical applications due to the formation of wide
particle size.
• 2. It is not easy to clean after use.
Roller Mill: Consists of two to five smooth rollers operating at different speeds. Size reduction is
due to compression and sheering action.
Colloid Mill: based on the Combined Impact and Attrition. Colloid mill works on the principle of
shearing. The colloid mill is useful for milling, dispersing, homogenizing and breaking down of
agglomerates. The material should be pre-milled as finely as possible to avoid damage to the
colloid mill and should be mixed with suitable liquid.
• The main function of the colloid mill is to ensure a breakdown of agglomerates or in the case of
emulsions to produce droplets of fine size around 1 micron.
• Construction : it consist of high speed rotor & stator with conical milling surface. milling surface
may be rough or smooth surface • Rough used for fibrous.
• The distance between rotor and stator is adjusted between 0.005
to 0.075 cm. The rotor is connected to a high speed motor which
can revolve at a speed of 3000 to 20000 rpm. The material is feed
to hopper and size of material is reduced as it passes through
moving rotor and stator.
• The material to be processed is fed by gravity to the hopper or pumped so as to pass
between the rotor and stator elements where it is subjected to high shearing and hydraulic
forces.
• The equipment breaks down materials by forming dispersion of materials in a liquid.
Shearing takes place in a narrow gap between a static cone (the stator) and a rapidly
rotating cone (the rotor).
• Material is discharged through a hopper whereby it can be re-circulated for a second
pass.
• For materials having higher solid and fiber contents conical grooved discs are preferred.
• To reduce wear, the rotor and stator are constructed using toughened steel or corundum.
• The rotor of a colloid mill can differ from one machine to another but the operating
principle is the same for all. Each manufacturer incorporates specific features that result
in changes in operating efficiency.
Advantages of Colloid Mills
• It has a wide range of use including comminution of slurry- fluid materials.
• The machine is simply constructed.
• It can be easily adjusted.
• Colloid mill is easy to clean after use
• The machine is self-draining.
• High capacity and minimal requirements.
• Reduced wear as a result of the construction of the rotor-stator with toughened steel/corundum.
• Low machine noise level.
Disadvantages of Colloid Mill
1. It has no wide application in solids
2. Wear of the rotating plates
3. No fine grinding
4. Consumes energy though still dependent on some factors.
Technique of milling
Special atmosphere: For hygroscopic material, in a closed system supplied with
dehumified air.
Thermolabile easily oxidizable and consumable material should be in a closed system with
an inert atmosphere.
Any fine dust mixture can be potential explosive under certain conditions especially is static
electrical charges result from the processing. All switches should be explosion proof and the
mill should be grounded.
Temperature control: Cooling by means of a cooling jacket or a heat exchanger. With
refrigerants, the mill should be of stainless steel as cast iron become brittle at low temp.
Waxy and low melting point materials are chilled before milling. Or materials can be mixed
with dry ice.
Pre-treatment: Sometimes pre-sizing is vital, Pre-treatment of fibrous material with high
pressure rolls or cutters facilitates communition.
Subsequent treatment: If extreme control of size is required, it may be necessary to
recycle the larger particles either by simply screening the discharge and returning the
oversize particles for a second milling or by using air separation equipment in a closed
circuit to return the oversized particles automatically to the milling camber. With material to
be reduced to micron size, an integrated air separation, conveyor and collection element
usually are required.