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ANALYTICAL

CHEMISTRY
(Gravimetry)
Dr.S.SURESH
Assistant Professor
Email:avitsureshindia@gm
ail.com

Gravimetric Analysis
Gravimetric analysis is the quantitative
determination of analyte concentration through a
process of precipitation of the analyte, isolation of
the precipitate, and weighing the isolated product.

Gravimetric Analysis
1. A weighed sample is dissolved
2. An excess of a precipitating agent is
added to this solution
3. The resulting precipitate is filtered,
dried (or ignited) and weighed
4. From
the
mass
and
known
composition of the precipitate, the
amount of the original ion can be
determined

Types of Crucibles
Different types of crucibles are used for
drying and weighing the precipitates.
They are mainly of two types.
Crucibles made of porcelain or silica are
used when the precipitates are dried in
an oven or muffle furnace.
Sintered
crucibles
are
used
for
precipitates which are weighed after
drying in air-oven.

Silica Crucible

Porcelain Crucible

Sintered Crucible

The degree of contamination in


gravimetric process
The types of contamination we come across in
gravimetry is

Co-precipitation and
Post-precipitation
Co-precipitation : Soluble impurities
which are getting precipitated along
with the formation of the precipitate.
Post-precipitation: After the formation
of the precipitate, the impurities will
get soluble.

Postprecipitation
Ca2+

(NH4)2C2O4

CaC2O4

If Mg2+ is present as an impurity in Ca2+, then we can have


a post precipitation of MgC2O4 over CaC2O4. The post
precipitation can be avoided by keeping a high pH.

Example for co-precipitation


When estimating barium
Ba2+ + SO42
Contaminated with CrO42-

BaSO4
BaCrO4

The contaminants will go and get occluded


inside the crystal lattice of BaSO4.
Co-precipitation can cause erroneous results.
In order to minimise this co-precipitation we
digest the precipitate.
Digesting the precipitate in suitable solvent
and reprecipitation gives good yield.

Gravimetric factor
A gravimetric factor converts grams of a
compound into grams of a single element.
Example: To find the gravimetric factor of Cl in
AgCl

AgCl

Ag

+ Cl

mass of Cl
Gravimetric factor Molecular
=
Mass of AgCl
35.5
143.3=

= 0.24

Gravimetric factor
Determine gravimetric factor of calcium in
water, if you precipitate calcium as CaCO 3.
Gravimetric factor =

Mass of Ca
Molecular Mass of CaCO3

= 40
100
= 0.4

Factors which affect solubility of


precipitate
Temperature: heat is absorbed as most
solids dissolve. Therefore the solubility of
precipitates increases with increasing
temperature.
Solvent composition: The nature of solvent
influences the solubility of most inorganic
substances
Diverse ion effect: Many slightly soluble
salts show an increased solubility in the
presence of increased concentration of
certain salts having no ion in common with
those of the slightly soluble salt.