PRECIPITATION

Definition:

It is a process of separating solid particles

from a previously clear liquid i.e., a solution, by
physical or chemical changes.
 The separated solid is called “Precipitate”,
 The cause of precipitation is called the
“precipitant” and
 The liquid which remains in the vessel above
the precipitate is called the “Supernatant liquid
or supernate”.
 Types of precipitates:
The terms curdy, granular, flocculant, gelatinous,
crystalline, bulky and others are used to define
the particular form which the precipitate attains
when it is thrown out of the solution.
The characteristic of the precipitate often
depends upon the conditions under which it has
been produced.
When the reacting substances are mixed at
temperature near to their boiling point the
precipitate is usually granular and heavy whereas
the precipitate of the same substance produced
by mixing cold solution may be light.
Factors affecting precipitation:
1. Nature of material
2. Light
3. Type of solvent
4. Temperature
5. Chemical reaction
6. Concentration of solution
7. Order of mixing
1. Nature of material:
If solution containing albuminous matter is heated, a
flocculant type of precipitate of coagulated albumin will
be formed.
2. Light:
If solution of silver nitrate is exposed to light,
precipitation will take place and precipitates are,
somewhat, curdy.
3. Type of solvent:
Crystalline precipitates are formed when alcohol or
alcoholic substances are added to a strong solution of
chemical salt. This is basically a chemical reaction and
many pharmaceuticals are formed by this method.
4. Temperature:
Some substances can be precipitated only from cold
solutions because low temperature reduces solubility of
salt and it precipitates out as a solid.

5. Chemical reaction:
Precipitates can form when two soluble salts react in
solution to form one or more insoluble products.

6. Concentration of solution:
Hot, dense solutions usually produce heavy precipitates
and these precipitates are readily washed from the
adherent matter than those which are light precipitates.
7. Order of mixing:
When different solutions are mixed, order of mixing has
to be followed. In some cases, the dissolved substances
are separated as precipitates that are not required. Also,
sometimes, the nature of precipitate changes by the
change of order.

Rule:

When in doubt, safe rule is to add the electropositive

element to the one with group of desired elements e.g.,
to get precipitates of lead sulphate, pour the solution of
lead compound to the one containing sulphate group.
 Method:
1. Formation of ppt:
Precipitation is usually carried out in heat resistant glass
beakers, and the solution of the precipitant is added
slowly and with efficient stirring.
The addition must always be made without splashing.
Only a moderate excess of reagents are added to
complete the precipitation.
As a general rule, precipitates are not filtered off
immediately. In most cases, they are allowed to stand
for 12-24 hours so that particles achieve the size which
can be easily filtered.
2. Filtration:
Filtration is the process of separating the ppt from the
mother liquor.
The systems employed for filtration are;
i) Filter paper
ii) Porous filter plates made of resistant glass, silica or
porcelain.
The choice of filtering media depends upon the nature
of ppt and cost.
3. Washing of precipitates:
Most precipitates are produced in the presence of one
or more soluble compounds. Since the soluble
compounds are frequently non-volatile at the drying
temperature of the ppt, so it is necessary to wash the
ppt to remove impurities as completely as possible.

Washing is done with minimum portion of liquid. It is

better to wash with a number of small portions of the
washing liquid, which are well drained between each
washing.
4. Drying and igniting precipitates:
After a ppt has been filtered and washed, it must be
dried before it can be weighed.
The drying and ignition process of the ppt will depend
on the nature of the ppt, the nature of the filtering
medium and the acceptable temperature to which the
ppt is heated.
In general, drying is applied when temperature is
below 250oC and ignition is applied up to 1200oC.
 Applications:

Precipitation has many applications:

1-It provides a convenient method of obtaining solid
substances in the form of fine particles e.g., ppt of CaCO3
(precipitated chalk).
2-One of the most important use of precipitation is in the
purification of solids. Process applied to purification is
termed recrystallization. The impure solid is dissolved in
a suitable solvent at elevated temperature. On cooling,
the bulk of the impurities remain solubilized while the
purified solid precipitates out.
3-Clarification of liquids through precipitation:
In many cases, part of the matter to be
removed, in order to get a clear product, is
formed by precipitation.
The important methods are:
i) ppt due to change of solvent
ii) ppt of proteins
iii) ppt by proteins (Adsorption)
i) Precipitation due to change of solvent:
 Whenever precipitation by change of solvent
is done, sufficient time of 12-24 hours is given for
solid particles to settle down and then separated by
filtration.
 Tinctures are usually clarified in this way, alternate
solvent may be water and alcohol.
ii) Precipitation of Proteins:
 The conversion of proteins into an insoluble form
and then removal by filtration may be considered as
a preliminary step to clarification.
 For example, Liquid extract of Liquorice, Pituitary
Extract, Purified Ox bile are obtained by this
technique.
iii) Precipitation by Proteins (adsorption):
 It has a limited application in Pharmacy
 e.g., it is used to remove tannins from wine and the
protein being used is gelatin. These substances swell
in cold water and form an adsorption compound
with tannins which is also insoluble and thus,
separated by filtration.
4-Purification of organic compounds:
The organic compounds derived from natural
sources are often mixed with other impurities.
Similarly the compounds prepared in the laboratory
are generally mixed with the by-products of
reaction. So, precipitation is performed for their
purification.
5-Precipitation reactions can be used for making
pigments.
6-For preparation of deionized water (for removing ions) that is used
in research experiments.

7-In classical qualitative inorganic analysis of different salts.

8-Precipitation reactions are used in the preparation of salts; in

qualitative analysis reactions; and in the formation of some
sedimentary rocks.

9-Identification of Blood Groups:

In vitro precipitation of blood (agglutination), on addition of a
foreign serum, is of utmost importance in confirming the presence
of a specific blood group or antigen.
10-Preparation of Sera for Blood Group Testing:
Whole Blood precipitation of cells (RBCs, WBCs,
Platelets) plasma Precipitation of coagulating
proteins (prothrombin, thrombin, fibrinogen) Serum