Abstract

This experiment is done to determine the percentage of ferum in a ferum solution. For
the determination, we have used the precipitate technique to get the mass of ferum. In
this part, gravimetric analysis is done by using filtration method to obtained the
filtrate. From this part, the filtrate formed is poured into crucible and it is heated at
300oC overnight to ensure that the filter paper have burnt completely to get the
precipitate. The precipitate is weighed to calculate the percentage of ferum in a ferum
solution.

Objective

To determine the percentage of Ferum in a Ferum solution

Introduction

Gravimetric analysis is defined as based upon the measurement of mass that can be
generali(ed into two types. Precipitation and volatilization are the types of this
gravimetric analysis. The quantitative determination of a substance by the
precipitation method of gravimetric analysis involves isolation of an ion in solution by
a precipitation reaction, filtering, washing the precipitate free of contaminants,
conversion of the precipitate to a product of known composition, and finally weighing
the precipitate and determining its mass by difference. From the mass and known
composition of the precipitate, the amount of the original ion can be determined.

In this technique! the analyte is converted to an insoluble form which can then be
washed, dried, and weighed in order to determine the concentration of the analyte in
the original solution. Gravimetry is applied to samples where a good precipitating
agent is available. The precipitate should be quantitative, easily washed and filtered
and is of in suitable quantity for accurate weighing. Therefore, gravimetry is regarded
as a macro analytical technique. However, it is considered, when appropriately done,
one of the most accurate analytical techniques. Also, Gravimetry is one of a few
analytical methods that do not require standard solutions as the weight of precipitate
is the only important parameter in analyte determination
The successful determination can be obtained by substance desired must be
completely precipitated. In most determinations the precipitate is of such low
solubility that losses from dissolution are negligible. For example

Fe2+ → Fe3+

Fe3+ + O2- → Fe2O3

The solubility of Fe2O3 is reduced still further by the excess of Fe3+ which is added,
pushing the equilibrium to the right. The weighed form of the product should be of
known composition. Since Fe2O3 is a stable compound, the mass of Fe in the solution
can be calculated.

Procedure

A. Preparing a crucible

The crucible was cleaned and heated for 10 minutes. It was then cooled in dessicator
and was accurately weighed.

B. Precipitation

25 mL Ferum solution is pipetted into a 400 mL beaker, 25 ml distilled water is

added and it is covered with watch glass. The solution is heated until it is boiled. 1 ml
concentrated nitric acid ,HNO3 is added by dropping it wisely. The solution is
continued heating until it became clear. The solution is diluted to 200 ml with distilled
water and it is boiled again. The beaker is transferred to the bench and 1:1 NH4OH is
slowly added into the solution and stirred until excessed. We noticed that is no more
formation of precipitate and the steam odour is smelled.

C. Filtering and washing the precipitate

The precipitate is filtered by decantation using the precipitation method for
gravimetric analysis without stirring the solution, so it ensured that most of the
precipitate will be left behind in the beaker. The precipitate was washed with 30 ml
warm 1% NH4NO3 solution. The solution is poured into the filter funnel leaving
behind most of the precipitate. The process is repeated for three times and finally all
the precipitates are quantitatively transferred into the funnel. Finally, the precipitate is
washed with warm distilled water and it is tested for chloride with acidic silver nitrate
solution.

D. Drying and weighing the precipitate

The filter paper that contained the filtrate is transferred into the crucible in above. The
crucible is heated by using a Bunsen burner with a small flame at the beginning until
all the paper burnt. The flame is increased and it is continued heating for another 20
minutes. The heating process is repeated until a constant mass is obtained. The
position of crucible is recorded on the piece of paper at the furnace. The precipitate
will be heated at 300oC overnight. When the crucible is cooled, the mass of precipitate
is weighed. The percentage of ferum is calculated.