LABORATORY REPORT

CHM421
(ANALYTICAL CHEMISTRY)

NAME: Irfan Nurhadi Bin Azahar

MATRIX NO.: 2020819572
GROUP: AS2222A1
EXPERIMENT TITTLE:Determination of Fe in a Ferum solution by Gravimetric Analysis
EXPERIMENT NO.: 8
DATE OF EXPERIMENT: 17 jun 2021
DATE OF REPORT SUBMISSION: 24 jun 2021
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 300 ̊C 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
1. To determine the percentage of Fe in a ferum solution

INTRODUCTION
Gravimetric analysis is defined as based upon the measurement of mass that can be generalized
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.
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. Precipitation

A 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 NH 4OH is slowly added
into the solution and stirred until it is excessed. We might notice that is no more
formation of precipitate and the steam odour is smelled.
B. Preparing a crucible

The crucible is cleaned and it is heated for 10 minutes. It is cooled in desiccator and it is
accurately weighed.

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 is washed with 30 mL warm 1% NH 4NO3 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 300 ̊C
overnight. When the crucible is cooled, the mass of precipitate is weighed. The
percentage of ferum is calculated.

RESULT & CALCULATION

Weight of empty crucible (g) 59.0843 59.0843 59.0843

Weight of crucible + precipitate (g) 59.2371 59.2320 59.2295
Weight of precipitate (g) 0.1528 0.1477 0.1452
Weight of precipitate (average), g = 0.1486
DISCUSSION

Before we entered the laboratory, we have made some preparation in the form of information
from the expected data. By using gravimetric method in calculation we calculated the value of
GF of Fe in Fe2o3 is 0.6994, weight of precipitate is 0.1486g and weight of analyte is 0.1039g. the
percentage fe in ferum solution is 0.4156%

CONCLUSION

1. The percentage of Ferum in Ferum solution obtained is 0.4156%

QUESTION

1. Why should the crucible be cooled before weighing?

- Hot objects would warm the air around would expand and would produce convection as it rises
causing to give the object a mass that is less than the actual.

2. What exactly happened to the filter paper during the ignition?

- decompose and filter paper is ashfree
3. What is the function of the nitric acid in the experiment?
- The nitric acid, along with boiling the solution, helps to precipitate the iron out
of the initial solution.