Desiccation

,sublimation &
tirturation
By: Dr. Tahseen
Ismail

Desiccation

Desiccation is the process of

removing adhered moisture from
liquid or solid substances. The term
"desiccated" should be used for those
substances from which water has
been completely removed.

Desiccation

Desiccation

On laboratory scale desiccation can be carried

out in a desiccator, which consists of a tightly
closed glass vessel containing a drying agent at
its bottom, which absorbs moisture from the
substance being desiccated. The commonly used
drying agents include concentrated sulphuric
acid, phosphorous pentoxide, exsiccated calcium
chloride and silica gel. The drug to be dried is
taken in a dish, which is placed inside the
desiccator above the surface of drying agent.
For continuous operation the desiccator may
sometimes be connected to a vacuum pump.

Desiccation

The substances which are very

sensitive to moisture are formulated
as tablets or capsules which are
further protected by enclosing them
in sealed vials, on the bottom of which
a small cloth bag containing silica gel
is placed which acts as a desiccant.

Desiccation

Applications
Desiccation helps in preserving the vegetable
and animal drugs which get destroyed in the
presence of moisture.
2. Comminution of drugs is difficult if they are
wet but if they are dry, can be easily powdered.
3. Desiccation reduces the bulk and weight of
the substances due to loss of adhering
moisture in them therefore they become easy
to handle.
4. Stability of certain drugs is also increased.

SUBLIMATION
Sublimation is the process in which
transforming the solid to vapors without
intermediate passage through the liquid
state.
Triple point.

Triple point is the point having a

definite temperature and pressure at
which the solid, liquid and vapor phases
of a chemical substance co-exist

Triple point is a point in a graph

between temperature and pressure at
which three phases like solid, liquid and

Method of sublimation

The pressure below the triple point is called as

Sublimation pressure.
In the diagram the line (AO) is known as
sublimation pressure. At this (O) point solid
and liquid are at equilibrium. If the sublimation
pressure is below this triple point the solid will
directly converted into vapor phase and the
vapor phase is directly change into solid.
Two factors in the diagram indicate that:
When the vapor pressure of the substance is
less then that of sublimation pressure, it will
directly change into solid or vapor phase
without changing into liquid phase.

Method of sublimation

When the vapor pressure of the substance

is high then that of the sublimation
pressure, then it will first convert into
liquid phase and then into solid state on
further cooling.
The common sublimed substances are as
follows:
Iodine
Naphthaline
Camphor
Para-dichloride benzene
Thus the vapor pressure of Iodine,
camphor, Naphthaline and p-dichloride
benzene are less triple point.

Method of sublimation

In laboratory it consists of a china dish, a

perforated filter paper, funnel, and a cotton plug.
The material to be sublimed is placed in the
china dish; the china dish is covered with a
perforated filter paper. A glass funnel is placed in
the inverted position over the filter paper; the
open end of the funnel is plugged with cotton to
prevent the escape of sublimed product.
The china dish is heated and vapors pass
through the perforations of the filter paper, and
are collected on the inner surface of the glass
funnel which is kept cool from out side by
wrapping a wet filter paper or cotton wool. The
vapors on cooling are condensed into solid which
is collected.

APPLICATIONS

This process is used in the

purification of many pharmaceutical
substances such as iodine, camphor,
naphthalene, benzoic acid, mercuric
chloride, ammonium chloride.
This process is also employed to
purify volatile solids contaminated
with non volatile impurities.

Trituration

By triturating the grinding of a solid substances is

done to fine powder by continuous strike in or
rubbing the particles in a mortar with a pestle.
The term trituration is also emloyed to designed
the process by which two or more powders are
intimately mixed with each other. For this purpose
a pestle and mortar made of, porcelain or glass is
used. For hard materials steel mortar and pestle
may be used.

Trituration may be carried out with a tile and

spatula or using a mortar and pestle.

Trituration using tile and

spatula

Small quantities of finely powdered solids may be

mixed on a tile by means of a spatula.
Tiles are usually made of glass and should be large
enough for the quantity of powder to be mixed or
ointment to be prepared. Usually for small scale work
300mm square is a useful size for a tile.
Spatula is made of stainless steel except for the few
medicaments those react with stainless steel (iodine),
should be flexible and long blade (25mm by200mm) to
provide a large rubbing surface.
Powders for Trituration are placed on the tile and
gently mixed until the mixture is smooth and
homogeneous, but in the case of ointment if base is
very soft it may be helpful to warm the tile but
overheating should be avoided because the base will
become too fluid and may run off the edge of the tile.
The dispersion is then diluted with increasing amount
of base, doubling the quantity each on the tile of each

Trituration using mortar &

pestle

A mortar should be used when the quantities are too

large . A mortar with a fairly flat base and a pestle
with a flat head will give best results.
It is impossible to ensure intimate dispersion of one
powder in another by mixing the two substances all at
once.
The purpose is to add a substance that is present in
greater amount to the whole of the substance present
in lesser amount. Substance present in greater
amount is introduced into the mixture in very small
quantities at first, but gradually increasing the
quantities, until the whole of the substance has been
added..