BP506-P INDUSTRIAL PHARMACY-I

SUPRIYA SAHU
BPH/10037/19

EXPERIMENT 09
AIM:
To prepare calcium carbonate granules using wet granulation technique

REFERENCE:
L. Kan.- The Theory and practice of Industrial Pharmacy, Leon Lachman,
Herbert A. Lieberman, Josephig, 3rd edition, page- 320

APPARATUS AND CHEMICALS:

Calcium Carbonate, lactose, starch paste, starch powder, talc, mineral oil,
mortar pestle, Sieve #10 or #12, hot air oven, measuring cylinder, hopper.

THEORY:
The wet granulation technique uses the same preparatory and finishing steps
(screening or milling, and mixing). The unique portions of wet granulation
process involve the wet massing of the powders, wet sizing or milling, and
drying. Wet granulation forms the granules by binding the powders together
with an adhesive, instead of by compaction. The wet granulation technique
employs a solution, suspension, or slurry containing a binder, which is usually
added to the powder mixture; however, the binder may be incorporated dry
into the powder mix, and the liquid may be added by itself.

The method of introducing the binder depends on its solubility and on the
components of the mixture. Since, in general, the mass should merely be moist
rather than wet or pasty, there is a limit to the amount of solvent that may be
employed. Therefore, when only a small quantity is permissible, the binder is
blended in with the dry powders initially; when a large quantity is required,
the binder is usually dissolved in the liquid.

The solubility of the binder also has an influence on the choice of methods,
since the solution should be fluid enough to disperse readily in the mass. The
liquid plays a key role in the granulation

process. Liquid bridges are developed between particles, and the tensile
strength of these bonds increases as the amount of liquid added is increased.
These surface tension forces and capillary pressure are primarily responsible
for initial granule formation and strength. Once the granulating liquid has
been added, mixing continues until a uniform dispersion is attained and all the
binder has been activated. During granulation, particles and agglomerates are
subjected to consolidating forces by action of machine parts and of
interparticulate forces. Granulation in large blenders requires 15 min to an
hour. The length of time depends on the wetting properties of the powder
mixture and the granulating fluid, and upon the efficiency of the mixer.

A rough way of determining the end point is to press a portion of the mass in
the palm of the hand; if the ball crumbles under moderate pressure, the
mixture is ready for the next stage in processing, which is wet screening.

A drying process is required in all wet granulation procedures to remove the

solvent that was used in forming the aggregates and to reduce the moisture
con- tent to an optimum level of concentration within the granules. During
drying, interparticulate bonds result from fusion or recrystallization and
curing of the binding agent, with Vander Waals forces playing a significant
role.

After drying, the granulation is screened again. The size of the screen depends
upon the grinding equipment used and the size of the tablet to be made.
PROCEDURE:

INGREDIENTS QUANTITY (mg)

Calcium Carbonate 100

Lactose (fine powder) 40

Starch paste 4
Starch (dry powder) 10
Talc 10
Mineral oil (50 ps) 4

1) Calcium carbonate and lactose are mixed homogenous mixture in dried

mortar pestle. We have to avoid aggressive mixture.

2) We added starch powder to calcium carbonate and lactose mixture.

3) We prepared a dough of the above mixture with starch paste (1-5 percent
is the concentration of the starch which can be potato or corn starch). It is
mixed in small quantity in mortar pestle and is observed that the entire
mixture can come in fist. It should not be too sticky nor too dry. On closing the
fist, it will form a lump which can be pressed with thumb to form a
compressed substance.

4) The compressed substance would break at the end point, if such happens
then there is no need to add further starch paste as excess of it can cause
hardening.

5) The compressed dough is then allowed to pass through sieve #10 or #12,
thereby, we would get granules, which is then transferred in a tube and placed
in hot air oven until they completely dry up and shows the free-flowing
property.
6) Before addition of talc and mineral oil, we evaluate the tap density, bulk
density, angle of repose and Carr’s index of the granule.

7) After the completion of evaluation, the talc is added. (Addition of talc is

avoided at times when there is obstruction in flow property of the obtained
granule). The talc quantity is then optimised and then the dried granule and
talc is mixed uniformly.

8) Mineral oil is then added to the obtained mixture.

9) After this process of granulation, the mixture is allowed to pass through

tablet punching machine which then further passes through hopper and dye
cavity and then finally the punching of the tablet is done.

EVALUATION:
Evaluation of dried granules is done before the addition of talc and mineral oil
and proceeding further. For the evaluation of granules, the bulk density, tap
density, angle of repose and Carr’s index of the granule is calculated
accordingly.

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