Lab 6 - Granulation of Powders

Philadelphia University
Faculty of Pharmacy
Industrial Pharmacy Practical
Granulation of Powders
Yasmeen Darwish
ydarwish@philadelphia.edu.jo
• Granulation is the process in which primary
powder particles are made to adhere to form
larger, multiparticle entities called granules.
• Pharmaceutical granules typically have a size
range between 0.2 and 4.0 mm, depending on
their subsequent use.
• In the majority of cases this will be in the
production of tablets or capsules, when
granules will be made as an intermediate
product and have a typical size range between
0.2 and 0.5 mm, but larger granules are used as
a dosage form in their own right
Advantages of granules over fine particles:
• Improve the flow properties.

• Improve the binding properties (compaction) among particles.
• Increase the density so decrease the volume of bulk powder.
• Controlled size and shape.
• Segregation of incompatible components.
• Controlled porosity.
• Reduction of dust hazards

Methods:
• Dry granulation:
• Some times known as "granulation by
preliminary compression". Lubricants are
added at the blending stage. There are two
main processes.
• Slugging: a large tablet (known as a 'slug') is
produced in a heavy-duty tabletting press
• Roller compaction: the powder is squeezed
between two rollers to produce a sheet of
material
• In both cases these intermediate products are broken
using a suitable milling technique to produce granular
material, which is usually sieved to separate the desired
size fraction. A hammer mill is suitable for breaking the
slugs while the sheets normally are weak and brittle
and breaks immediately into flakes by screening.

• The chief advantage of this method is that it eliminates
heat and moisture and hence can be applied to
hydrolysable compounds, which would decompose
during moist granulation. The disadvantage is that
there is a tendency to produce a high proportion of
fines. The unused fine material may be reworked to
avoid waste
• Dry binder …………. PVP (Poly vinyl pyrolidone )
Wet granulation:
The most widely and most commonly used
granulation technique although it involves so
many separate steps which require time,
laboratory work and cost. Heat and/or moisture
sensitive drugs are affected by this method, yet,
for poorly cohesive powder, it is the method of
choice.
Steps:
• Weighing……….excipient + a.i
• Mixing
• Wet massing……….addition g.f (planetary mixer)
• Screening (oscillating granulator )…. Wet granule
• Drying….oven , fluidized bed dryer
• Dry screening( sieving)
• Lubrication
• Compression
 Wet massing……….addition g.f
• G.f ……….solvent
• G.f ………… solvent+ adhesive binder
• (binder sol)….. 1- sucrose sol
• 2- starch mucilage
• 3- acacia mucilage
• 4- gelatin sol
• The most critical step:
• If g.f higher than optimum …..
• 1- very hard granule : difficult to be compressed , delay disintegration
and dissolution
• If add in % lower than optimum:
• Too soft , fragile ………. Difficult to be compressed
• End point ………. Coherent damp mass
• Snow damp mass
• Brown sugar damp mass
granulating fluid:
• The fluid contains a solvent which must be volatile so that it can be
removed by drying, and be non-toxic.
• Typical liquids include water, ethanol and isopropanol, either alone or in
combination.
• The granulation liquid may be used alone or, more usually, as a solvent
containing a dissolved adhesive (also referred to as a binder or binding
agent) which is used to ensure particle adhesion once the granule is dry.
• The powder mass is wetted with the binder solution until the mass has
the consistency of damp snow or brown sugar. If mass is over wetted,
this will result in the hardness off granules and so, more pressure is
needed to compress tablets which are difficult to disintegrate or
dissolute. If it is not wetted sufficiently, the resulted granules will be too
soft and break during lubrication and compression.
• After formation of the wet mass, it is passed through a screen then the
granules are dried.
Interfacial forces in mobile liquid films:
• At low moisture levels, termed the pendular state, the particles are held
together by lens-shaped rings of liquid.
• These cause adhesion because of the surface tension forces of the
liquid/air interface and the hydrostatic suction pressure in the liquid
bridge.
• When all the air has been displaced from between the particles the
capillary state is reached, and the particles are held by capillary suction
at the liquid/air interface, which is now only at the granule surface.
• The funicular state represents an intermediate stage between the
pendular and capillary states. Moist granule tensile strength increases
about three times between the pendular and the capillary state.
•
• It may appear that the state of the powder bed is dependent upon the
total moisture content of the wetted powders, but the capillary state
may also be reached by
• decreasing the separation of the particles. In the massing process during
wet granulation, continued kneading/mixing of material originally in the
pendular state will densify the wet mass, decreasing the pore volume
occupied by air and eventually producing the funicular or capillary state
without further liquid addition.
• These wet bridges are only temporary structures in wet granulation
because the moist granules will be dried. They are, however, a
prerequisite for the formation of solid bridges formed by adhesives
present in the liquid, or by materials that dissolve in the granulating
liquid
Procedure:
• Weigh 400g of lactose and transfer to the planetary mixer
then add sufficient amount of distilled water and mass for
5 minutes. The water should be added gradually and the
formation of the damp coherent be tested after each
addition/mixing step.
• Remove the wet mass and pass through 1.4 mm sieve

fitted to the oscillating granulator. Collect the granules on
a stainless steel pan and spread to form a thin bed off
granules.
• Dry the granules in the oven at 70° C for 45 minutes.

Note: An alternative method of drying is fluidized bed
drying; the lab instructor will provide you with the
required instructions for this step.
• Screen the granules through a sieve of smaller size.
(granules A)
• Repeat the steps using sucrose solution instead of

distilled water.(granules B)
• Repeat the steps using 350g lactose and 50g of

acetyl salicylic acid and enough starch mucilage as
granulating agent.(granules C)
• Keep the granules for the subsequent lab.

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Philadelphia University

• Improve the flow properties.

• Remove the wet mass and pass through 1.4 mm sieve

• Dry the granules in the oven at 70° C for 45 minutes.

• Repeat the steps using sucrose solution instead of

• Repeat the steps using 350g lactose and 50g of

• Keep the granules for the subsequent lab.

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