GRAVIMETRIC ANALYSIS STEPS IN GRAVIMETRIC ANALYSIS

after the sample has been dissolved, can be

GRAVIMETRIC ANALYSIS summarized as follows:
➢ quantitative methods that are based on 1. Preparation of the Solution
measuring the mass of a pure compound to o It involves several steps including
which the analyte is chemically related. adjustment of the pH of the solution in
➢ gravimetric analysis is potentially one of the order for the precipitate to occur
most accurate classes of analytical methods quantitatively and get a precipitate of
desired properties, removing
TYPES OF GRAVIMETRIC ANALYSIS: interferences …etc.
Precipitation ➢ the analyte is separated 2. Precipitation
from a solution of the o this requires addition of a precipitating
sample as a precipitate and agent solution to the sample solution.
is converted to a compound o Upon addition of the first drops of the
of known composition that precipitating agent, supersaturation
can be weighed occurs, then nucleation starts to occur
Volatilization ➢ the analyte is separated where every few molecules of
from other constituents of a precipitate aggregate together forming
sample by conversion to a a nucleus.
gas . o At this point, addition of extra
o The weight of this gas precipitating agent will either form new
then serves as a nuclei (precipitate with small particles)
measure of the analyte or will build up on existing nuclei to give
concentration a precipitate with large particles ..
Electrogravimetry ➢ the analyte is separated by o The size of the precipitate can be
deposition on an electrode predicted by the Von Weighmann ratio:
by an electrical current.
o The mass of this
product then provides a
measure of the analyte
concentration.

PRECIPITATION
o In precipitation gravimetry, the analyte is
converted to a sparingly soluble precipitate.
o This precipitate is then filtered, washed free of
impurities, converted to a product of known
composition by suitable heat treatment, and
weighed.
o For example, a precipitation method for
determining calcium in natural waters involves
the addition of C2O4 2- as a precipitating agent

o The precipitate CaC2O4 is filtered, then dried

and ignited to convert it entirely to calcium
oxide

o After cooling, the precipitate is weighed, and

the calcium content of the sample is then
computed
3. Digestion of precipitate The following are ways that a precipitate can be
o Known as Ostwald ripening contaminated and should be avoided:
o The precipitate is left hot (below • Coprecipitation
boiling) for 30 min to 1 hour in order for o This is anything unwanted which
the particles to be digested. precipitates with the analyte during
o Digestion involves dissolution of small precipitation.
particles and reprecipitation on larger o Coprecipitation occurs to some degree
ones resulting in particle growth and in every gravimetric analysis (especially
better precipitate characteristics. barium sulfate and those involving
hydrous oxides).
4. Washing and Filtering o You cannot avoid it all what you can do
o Reduces problems with surface is minimize it by careful precipitation
adsorption and thorough washing
o Peptization occurs during washing • Surface adsorption
o Peptization: process by which a o Here unwanted material is adsorbed
coagulated colloid reverts to its original onto the surface of the precipitate.
dispersed state o Digestion of a precipitate reduces the
o in case of colloidal precipitates do not amount of surface area and hence the
use water as a washing solution since area available for surface adsorption.
peptization would occur. o Washing can also remove surface
o In such situations dilute volatile material.
electrolyte such as nitric acid, • Occlusion
ammonium nitrate, or dilute acetic acid o This is a type of coprecipitation in which
may be used. impurities are trapped within the
growing crystal.
5. Drying and Ignition: o Can be reduced by digestion and
o The purpose of drying (heating at about reprecipitation
120-150°C in an oven) is to remove the • Post precipitation
remaining moisture o Sometimes a precipitate standing in
o The purpose of ignition in a muffle contact with the mother liquor
furnace at temperatures ranging from becomes contaminated by the
600-1200°C is to get a material with precipitation of an impurity on top of
exactly known chemical structure so the desired precipitate.
that the amount of analyte can be o To reduce post precipitation filter as
accurately determined. soon as the precipitation is complete
o The precipitate is converted to a more and avoid digestion
chemically stable form.

6. Weighing the precipitate

Precipitating Agents
o The precipitate cannot be weighed with ➢ Ideally a gravimetric precipitating agent should
the necessary accuracy in place on the react specifically or at least selectively with the
filter paper; nor can the precipitate be analyte
completely removed from the filter ➢ Specific reagents which are rare, react only with
paper in order to weigh it. a single chemical species.
o The precipitate can be carefully heated ➢ Selective reagents which are more common,
in a crucible until the filter paper has react with a limited number of species
burned away; this leaves only the ➢ In addition to specificity and selectivity, the
precipitate. ideal precipitating reagent would:
o "ashless" paper is used so that the o react with analyte to give a precipitate
precipitate is not contaminated with that has the preferred requirements
ash. which have been previously discussed
o If you use Goosh crucible then after the
precipitate is allowed to cool Precipitating Agents
(preferably in a desiccator to keep it Inorganic ➢ Inorganic precipitating agents :
from absorbing moisture), it is weighed ➢ The inorganic precipitants e.g. S2- ,
(in the crucible) CO3 2- , PO4 3- …etc. are usually not
selective compared to the organic
precipitants but it give precipitates
with well known formula .
Organic ➢ The organic precipitants such as
dimethglyoxime and 8-
 hydroxyquinoline are more selective
than inorganic precipitants .
➢ They produce with the analyte less
soluble precipitate (small Ksp ) .
➢ They also have high molecular
weight so that the weighing error is
reduced.
➢ disadvantage of organic
precipitants is that they usually
form with the analyte a precipitate
of unknown formula

Calculation of Results from Gravimetric

Data
The results of a gravimetric analysis are generally
computed from two experimental measurements:
o the weight of sample
o the weight of a known composition precipitate

Determine the gravimetric factors (GF) for

the following:

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