GRAVIMETRIC ANALYSIS
Gravimetric analysis is based on the measurement of the weight of an analyte or of
a compound of known composition that contains the analyte.
Precipitation: In gravimetric precipitation, an analyte (the substance being
measured) is transformed into an insoluble compound by adding a reagent
that causes it to precipitate out of solution. The precipitate is then filtered,
washed, dried (or ignited to remove any volatile components if needed), and
weighed. The weight of this pure compound is used to calculate the amount
of the analyte. The precipitate is dried to a constant, reproducible mass to
ensure the solid has no longer absorbed water from the air and increased in
weight.
Volatilization: In the volatilization method, the analyte is converted into a
gaseous form, which is then measured indirectly by collecting and weighing
the residue or directly by weighing the amount of gas lost.
For successful determinations, the precipitate must:
Have a sufficiently low solubility so that losses from dissolving are
negligible
Be of known composition after drying
Easily filtered
Readily washed free of impurities
Not react in the atmosphere
Have a high purity
Gravimetric Apparatus
1. Suction Flask
A suction flask (also known as a Büchner flask or vacuum flask) is a heavy-
walled flask used with a vacuum source to create suction.
Its purpose is to assist in the filtration process by pulling liquid through a
filter more quickly than gravity alone would allow.
The side arm on the flask connects to a vacuum pump or aspirator, helping
to dry the precipitate faster by reducing the pressure and increasing the
filtration rate.
2. Suction Funnel
A suction funnel, often a Büchner funnel (for paper filters) or a sintered
glass funnel (for finer particles), is used in conjunction with a suction flask
for rapid filtration.
The funnel holds the precipitate on its filter medium (filter paper or sintered
glass disk) while the vacuum draws liquid through it, leaving the solid
precipitate behind.
This setup ensures efficient separation of the precipitate from the liquid
phase, which is essential for accurate weighing in gravimetric analysis.
3. Silica Crucible
A silica crucible is a heat-resistant container used to heat samples at high
temperatures, often above 1000°C, without contamination.
Its high thermal stability and resistance to chemical attack make it ideal for
drying or igniting precipitates to constant weight.
Silica crucibles are used especially in applications where volatile materials
must be removed or samples must be converted to a stable form for precise
weighing.
4. Sintered Glass Crucible
A sintered glass crucible has a porous glass bottom that serves as a built-in
filter for fine precipitates.
It allows for easy filtration without needing filter paper, which can introduce
impurities.
After filtration, the crucible can be dried or heated gently to remove
moisture from the precipitate, making it useful for gravimetric
determinations that require the precipitate to remain in the crucible for
weighing.
5. Oven
An oven is used to dry samples at controlled temperatures, typically between
100°C and 200°C, to remove moisture or volatile impurities without causing
chemical decomposition.
It ensures that the precipitate reaches a constant weight, a crucial step in
gravimetric analysis, as even slight moisture can affect accuracy.
Ovens are commonly used for drying precipitates before they are weighed or
further heated in a furnace if higher temperatures are needed.
6. Furnace
A furnace is used to heat samples to very high temperatures, often exceeding
1000°C, for processes like ashing, igniting precipitates, or converting them
into a stable oxide form.
It ensures complete volatilization of unwanted compounds or chemically
stabilizes the sample to obtain a residue that can be accurately weighed.
Furnaces are especially useful in analyses requiring high-temperature
treatments, such as the removal of organic matter or the conversion of metals
to oxides.
Gravimetric General Method
1. The sample to be analyzed (analyte) is weighed on an electronic balance
2. Analyte is dissolved in a solvent such as water
3. The precipitating reagent is added in excess to precipitate out the analyte
4. The resulting precipitate is filtered off (using a Buchner/suction funnel and
flask for faster filtration)
5. Precipitate is washed with distilled water to remove impurities
6. Precipitate is heated in crucible to remove added water
7. Precipitate is cooled in a desiccator to prevent moisture form the air from being
absorbed.
8. The cooled precipitate is weighed
9. Steps 7 and 8 will be repeated until a constant mass is achieved
[Link] percentage of analyte in the sample is then calculated
SOE:
1. If precipitating reagent is not added in excess, some of the analyte will
remain in soluble form.
2. If crystals are not properly dried, excess weight
3. Other ions may be precipitated, excess weight
