LABORATORY REPORT

CHM421
(ANALYTICAL CHEMISTRY)

NAME:
STUDENT NO.:
GROUP: AS2464A1
EXPERIMENT NO: 8
EXPERIMENT TITLE: DETERMINATION OF Fe IN A FERUM SOLUTION BY
GRAVIMETRIC ANALYSIS

ABSTRACT
This experiment was carried out to determine the percentage of Ferum in a Ferum Solution. The
method used in order to determine the Ferum was precipitation technique. In order to calculate
the percentage of Ferum, it was calculated using gravimetric analysis. The result in this
experiment in the term of Ferum % (w/v) is 0.421% (w/v).

OBJECTIVE
To determine the percentage of Ferum in a Ferum Solution

METHOD
A. Precipitation
25.0 mL ferum solution was pipetted into a 400 mL beaker, 25 mL of distilled water was
added and covered with watch glass. The solution was heated to boiling. 1 mL concentrated
HNO3 was added dropwisely. The heating continued until the solution became clear. The
solution was diluted to 200 mL with distilled water and the solution was boiled again. The
beaker was transferred to the bench and 1:1 of NH4OH was added into the solution slowly
and stirred until it was in excess.

B. Preparing a crucible
The crucible was cleaned and heated for 10 minutes. Cooled it in a desiccator and weighed
it accurately.

C. Filtering and washing the precipitate

The precipitate was filtered by decantation using filter paper no. 41 without stirring the
solution.the precipitate was washed with 30 mL warm 1% NH4NO3 solutions. The solution
was poured into the filter funnel leaving behind most of the precipitate. The same step was
repeated another two times and all the precipitate was transferred quantitatively into the
funnel. The precipitate was washed in the funnel using warm distilled water and the filtrate
was tested for chloride with acidic silver nitrate solution.

D. Drying and weighing the precipitate

 The filter paper containing all the precipitate was transferred into the crucible. The crucible
was heated using a Bunsen burner with a small flame at the beginning until all the paper
had burnt. The flame was increased and continued heating for 20 minutes. The heating
process is repeated until a constant mass is obtained. Place the crucible containing the
precipitate and filter paper at the furnace if the time does not permit. The precipitate was
heated at 300 C overnight. Weigh the mass of the precipitate once the crucible was cooled.

RESULT
Weight of empty crucible (g) 59.0843 59.0843 59.0843
Weight of crucible + precipitate 59.2371 59.2320 59.2295
(g)
Weight of precipitate (g) 0.1528 0.1477 0.1452

Weight of precipitate (average), g = 0.1486

Gravimetric factor (GF) ×

Weight of Fe = GF × weight of weighing form

= 0.6994 × 0.1486g
= 0.1039g

Percentage % (w/v) analyte

= 0.42 % w/v
DISCUSSION
In this experiment, the ferum solution was used as an analyte in order to determine the percentage
of Ferum in the Ferum Solution. Gravimetric analysis was used in this experiment. There are four
parts of the method used. In part A, the Ferum solution, distilled water as well as the concentrated
HNO3 was heated until the solution was clear. Then, the heating and dilution process was done,
NH4OH was added to solution until all the precipitate disappeared. For the next part, the crucible
was cleaned, heated, cooled and weighed. Using the filter paper and 1% NH4NO3 solution, the
precipitate was filtered and washed using it. Before the filtration for chloride with the acidic silver
nitrate solution was done, the filtered precipitate was washed using warm water. Next the last part
is the precipitate was dried and weighed using an ignition process on filter paper, then heated at
300 ˚C overnight and weighed the mass.

The result in this experiment was that Fe(II) was oxidized to Fe(III) and ferric oxide hydrates,
Fe2O2XH2O precipitate, were formed. Then, after filtering, washing, drying and weighing of the
precipitate, the precipitate was formed as ferric oxide, Fe2O3. The equation was:

Fe2+ → Fe3+
Fe3+ + O2- → Fe2O3

The average weight of the Fe2O3 precipitate was 0.1486g. The gravimetric analysis done was
0.6994. The weight of Fe in this experiment was 0.1039g and the percentages % (w/v) of Ferum
in this experiment was 0.42 % w/v.

The precaution in this experiment was when handling the NH4OH, always use gloves, a mask,
goggles, and a lab coat to avoid hazard since the NH4OH produces an unpleasant odour and can
make breathing difficult. Other than that, make sure the eye’s level must be perpendicular to avoid
parallax error. Last but not least, keep the analytical balance calibrated before use.

CONCLUSION
In conclusion, the objective, to determine the percentage of ferum in a ferum solution was
achieved. The percentages % (w/v) of Ferum in Ferum solution was 0.42 % w/v.

REFERENCES 1. 7: Gravimetric Analysis (Experiment). (2017, November 26). Chemistry

LibreTexts.

https://chem.libretexts.org/Ancillary_Materials/Laboratory_Experiments/Wet_Lab_Exper

iments/General_Chemistry_Labs/Online_Chemistry_Lab_Manual/Chem_11_Experiment

s/07%3A_Gravimetric_Analysis_(Experiment)

2. Erdey, L. (2013). Gravimetric Analysis: International Series of Monographs on

Analytical Chemistry, Vol. 7 (Vol. 7). Elsevier.

3. HARGIS L.G, Analytical Chemistry , principle and techniques, 1998

QUESTIONS
1. Why should the crucible be cooled before weighing?
There is no moisture coating on the crucible while it is heated. However, as the crucible
cools, moisture from the air condenses on it, altering its weight. This can cause inaccurate
reading to the weight of crucible.

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

During ignition, the crucible was heated to specific temperature thus the filter paper was
converted to water and carbon dioxide in the term of gaseous.

3. What is the function of the nitric acid in the experiment?

Function of nitric acid is to assist in precipitation of iron from solution.