Gravimetric Analysis

Qualitative analysis: Identification the components at a given substance.

Quantitative analysis: Determination of the concentration of the individual
elements or compounds present in a substance.
The Principle of Gravimetric Analysis:
In gravimetric analysis: - The percentage of a given ion in a substance is usually
found from the weight of a weighted formed when the element or ion is converted
into precipitated form and ignited to the most stable structure.
The Precipitated Form:
is the name given to the compound precipitated from solution by the action of the
appropriate reagent.
1- Fe3+ Fe(OH)3 2- Al3+ Al(OH)3 3- SO42- or Ba2+ BaSO4
Physical properties of precipitates:
1- The Precipitated form should have low solubility Ksp less than 10 8-
2- the precipitate should be such as to allow of rapid filtration and washing
3- the precipitated form must be converted easily and completely into the
weighed form.
The Weighed From:
is the compound, which is weighed for determinations of the result.
1- Fe3+ Fe2O3 2- Al3+ Al2O3 3- SO42- or Ba 2+ BaSO4
Physical properties of the weighed form
1- has definite and known structure.
2- Stable does not decompose or doesn’t affect by moisture and sunlight.
3- Give large yield thus it Can be detected
Problems (Disadvantages) in precipitation
Coprecipitation: The precipitate is usually found contaminated with substances, or
(Prescence impurities with the precipitate) which are normally soluble under the
conditions of the precipitation. This is called coprecipitation and is caused by
adsorption or occlusion.
Adsorption: In this contaminates (impurities) are present on the surface of the
particles of the precipitate.
To minimize Adsorption:
1- addition of 2-3ml conc HCl. 2- Dilute solution to 150 ml
3- Warm the solution before precipitation (raising temperature)
4- The reagent should be added slowly in small portions to the solution of the
sample with constant stirring in constant temperature.
Occlusion: When the impurities are found deep into the interior(bulk) of the
aggregate particles of the precipitates.
To minimize Occlusion:
1- The precipitate is warmed and allowed to stand with the hot mother liquor
for few hours; this is termed digestion.

Post-precipitation: the secondary precipitation of a foreign substance on the

particles of the primary precipitate, when calcium is precipitated as calcium
oxalate in presence of magnesium, magnesium oxalate is post-precipitated on the
crystals of calcium oxalate.
To minimize post-precipitation:
Reprecipitation is sometimes necessary to eliminate post-precipitation. The
precipitate first formed is filtered and dissolved in an acid and then precipitated
again
Peptization: The redispersion of the coagulated precipitate to form a colloidal
solution
To minimize Peptization
The precipitate should be washed with a dilute solution of a suitable electrolyte
such as ammonium nitrate in order to inhibit peptization.
Why addition of concentrated HCl before precipitation?
1- To solubilize impurities and this leads to inhibition of adsorption.
Classify or write-down the types of precipitates?
1-Crystalline ppt 2- Colloidal or gelatinous ppt
BaSO4 is crystalline ppt needs digestion process and washed by hot distilled
water, While Fe(OH)3 and Al(OH)3 doesn’t need digestion process and washed by
weak electrolyte (NH4NO3).
Write the property of filter paper must be used in gravimetric analysis and why?

1- The filter paper must be ashless (empty from carbon) to volatilize easily
2- and presence of the filter paper carbon, the reduction takes place even at
600° (BaSO4 + 4C = BaS + 4 CO).
Explain Why washing of Fe(OH)3 with NH4NO3 NOT NH4Cl?
To avoid peptization of ppt and converting to soluble compounds
Fe(OH)2Cl and Fe(OH)Cl2
Explain Why Addition of concentrated nitric acid with boiling in precipitation of
Fe2+?
To oxidize Fe2+ to Fe3+ because ferric is more stable than ferrous.
Explain Why filtration of ferric hydroxide on hot?
Because Fe(OH)3 is a gelatinous ppt on cooling cause blocking of filter paper, so
it is filtered on hot.
Discuss the test for complete precipitation?
Place a drop of freshly prepared solution of potassium ferricyanide K3[Fe(CN)6]
on a clean filter paper and add another drop of the solution in the beaker and
touch it with the ferricyanide drop. If no blue or green color appears the oxidation
is complete.

Desiccator: A desiccator is used or holding crucibles to protect then and their

contents from moisture. usually contains anhydrous calcium chloride.

Good Luck