Unit 2 Module 2

Gravimetric Analysis
Precipitation method 1 of 4
•In most cases, the analyte must first be converted to a
solid by precipitation with an appropriate reagent.
The precipitate can then be collected by filtration,
washed, dried to remove traces of moisture from the
solution, and weighed. The amount of analyte in the
original sample can then be calculated from the mass
of the precipitate and its chemical composition.
Precipitation method 2 of 4
•When the precipitating reagent is added, there is a period of
induction (time taken before the first sign of precipitate is
seen) and then nucleation (when a minimum amount of ions
come together to form a stable solid) occurs. Large crystals
are preferred to small crystals as they are more easily
filtered, digestion (heating of the solid and mother liquor
[liquid containing the solid]) encourages the formation of
large crystals.
Precipitation method 3 of 4
• For filtration, a vacuum pump is
used (large conical flask
connected to a tap via an
aspirator), sintered crucible are
used (small crucible with very
high melting point) which can
withstand high pressures used in
vacuum filtration. A rubber
policeman (glass rod with a hard
rubber scrapper on one end) is
also used to transfer residues of
solid or precipitate onto glass
surfaces.
Precipitation method 4 of 4
• The filtrate is tested with an
appropriate reagent to ensure
precipitation is complete. The
precipitate is rinsed with cold
distilled water and then heated
in an oven to remove all traces
of water and then cooled in a
dessicator before weighing. In
some cases ashless filter paper
can be used and the precipitate
heated and the filter paper
burnt away to leave just the
precipitate behind.
Volatilisation method 1 of 2
• In other cases, the volatilisation
method would be used. For
example, you are given a hydrated
salt and the object is to determine
the number of moles of water of
crystallisation present. It would be
heated to remove the water and the
difference in mass can then be used
to determine the amount of water
present and thus the number of
moles of water needed for one mole
of the anhydrous salt.
 Types of volatilisation methods
• Direct
Water eliminated in a quantitative manner
from many inorganic substances by ignition water by measuring the loss in mass
is an example of a direct determination. It is
collected on a solid desiccant and its mass
determined by the gain in mass of the
desiccant.
• Another direct volatilization method
involves carbonates which generally
decompose to release carbon dioxide when
acids are used. Because carbon dioxide is
easily evolved when heat is applied, its mass
is directly established by the measured
increase in the mass of the absorbent solid
used.
• Indirect
Determination of the amount of
of the sample during heating is an
example of an indirect method. It is
well known that changes in mass
occur due to decomposition of many
substances when heat is applied,
regardless of the presence or absence
of water. Because one must make the
assumption that water was the only
component lost, this method is less
satisfactory than direct methods.
Volatilisation method 2 of 2
• In other cases, the volatilisation
method would be used. For
example, you are given a hydrated
salt and the object is to determine
the number of moles of water of
crystallisation present. It would be
heated to remove the water and the
difference in mass can then be used
to determine the amount of water A rubber policeman
present and thus the number of
moles of water needed for one mole
of the anhydrous salt.
VIDEOS
• VIDEO OF GRAVIMETRIC ANALYSIS OF A CHLORIDE SALT
Applications of gravimetric analysis
• Measurement of the “essential” elements in plant foods (phosphorus,
is converted into the insoluble salt, magnesium ammonium
phosphate)
• Estimation of pollutants in the air, such as sulphur dioxide (by
conversion to insoluble barium sulphate)
• Estimation of sulphur dioxide (used to prevent microbial spoilage) in
soft drinks, such as orange juice.
• Estimation of chloride ions in water supplies (by conversion to
insoluble silver chloride).
Practice Questions 1 of
• The following is an excerpt from the laboratory report of the method used by a
student used to prepare a substance, S, for gravimetric analysis. “Two solutions
were mixed to produce a precipitate of S. S was obtained by quickly filtering the
mixture. The residue S was then washed with THREE consecutive 20 cm3
volumes of distilled water. S was then strongly heated for 15 minutes and then
allowed to cool to room temperature and weighed. The heating and cooling
process was repeated until constant mass was achieved.”
• a) State the purpose of
• i) Washing the residue with distilled water
• ii) Repeatedly heating and cooling until constant mass is achieved
• b) State TWO pieces of apparatus that would be required to obtain and rinse
the residue.
Practice Questions 2 of
• Washing soda is hydrated sodium sulphate, Na2SO4.xH2O. A sample
of washing soda was heated in a crucible to constant mass.

• The following observations were made

• mass of crucible = 34.25 g
• mass of crucible and washing soda = 40.69 g
• mass of crucible and washing soda after heating = 37.09 g

• Calculate the value of x in the formula Na2SO4.xH2O.

Ar Na = 23, S = 32, O = 16, H = 1