FACULTY OF APPLIED SCIENCES

LABORATORY REPORT

ANALYTICAL CHEMISTRY
(CHM 421)

Name of student Amirah Ishami Binti Ishak

Matrix Number 2022835624

Course code AS245

Title of the experiment Determination of Fe in a Ferum Solution by

Gravimetric Analysis

Experiment number Experiment 8

Instructor’s (lecturer’s) name Dr. Mohd Azizi Nawawi

Date of the experiment 8/12/2022

Abstract
This experiment is was carried out in order to determine the percentage of ferum in a ferum
solution using precipitate technique (Gravimetric Analysis) to get the mass of ferum from a
filtrate. A crucible was weighed together with its lid and was heated in a furnace for 10 minutes.
Then it was cooled in dessicator and weighed accurately. 25.0 mL of Fe solution was pipetted into
400 mL beaker followed with 25 mL of distilled water and cover with watch glass. Boiling process
then takes place while l mL of concentrated HNO3 was added dropwisely until the solution becomes
clear. Next, the solution was diluted to 200 mL with distilled water and boiled again. The beaker was
transferred to the fume cupboard and 1:1 NH4 OH was added slowly with stirring, until reached
excess state. Then 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. With this way we can
obtain the weight of precipitate in the determination of Fe in a Ferum solution. The precipitate was
weighed of 0.0322 g. The percentage of ferum in the solution can also be calculated which is 0.09%.

Objectives
1. To determine the percentage of ferum in a ferum solution.

Introduction
Gravimetric analysis is a method that will be used to determine a substance’s mass or concentration
by measuring changes in mass. Behind the principle of the gravimetric analysis is the mass of an ion
in a pure compound that can be determine. The mass of this ion later will be used to find the mass
percent of the same ion in a known quantity of an impure compound. Gravimetric analysis allows for
highly detailed analysis if procedures were done precisely. As a matter of fact, gravimetric analysis
can be used to calculate the atomic masses of specific elements in periodic table to six figure
precision. There are four fundamental types of gravimetric analysis which are volatilization
gravimetry, precipitation gravimetry, electrogravimetry and thermogravimetry.

In this experiment, we will determine the concentration of Fe in a given solution. Fe(II) will oxidised
to Fe(III) and then precipitated as ferric oxide hydrates, Fe2 O3 . XH2 O. The precipitate was filtered,
washed and dried to produce ferric oxide, Fe2 O3 . Since Fe2 O3 is a stable compound, we need to
calculate the mass of Fe in the solution.

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+ + e-

2Fe3+ + 3O2- → Fe2 O3

Method

A. Preparing a Crucible
In Part A, a crucible was cleaned with its lid and it was heated in a furnace for 10 minutes. It was
cooled in a desiccator and accurately weighed.

B. Precepitation
A 25 mL Ferum solution was pipetted into a 400 mL beaker, 25 mL distilled water was added and it
was covered with watch glass. The solution was heated until it is boiled. A 1 mL of concentrated
HNO3 was added and dropped wisely. The solution was continued heating until it became clear. The
solution was diluted to 200 mL with distilled water and it was boiled again. The beaker was
transferred to the fume cupboard and 1:1 NH4 OH was slowly added into the solution and stirred
until it was in excessed. We might notice that there is no more formation of precipitate and when
the steam odour was smelled.

C. Filtering and Washing the Precipitate

The precipitate was filtered by decantation using filter paper no. 41 without stirred the solution to
ensure that most of the precipitate would be left behind in the beaker. Then the precipitate was
washed with 30 mL of warm 1% NH4 OH solutions. The solution was poured into the filter funnel
leaving behind most of the precipitate. The process was repeated for another two times and finally
all the precipitates are quantitatively transferred into the funnel. Finally, the precipitate in the
funnel was washed with warm distilled water and the filtrate was tested for chloride with acidic
silver nitrate solution.

D. Drying and Weighing the Precipitate

The filter paper that contained all the precipitate was transferred into the crucible that have been
prepared. The crucible was heated using a Bunsen burner with a small flame at the beginning until
all the paper burnt. The flame was increased and continued heating for another 20 minutes. The
heating process was repeated until a constant mass was obtained. The position of crucible was
recorded on the piece of paper at the furnace. The precipitate will be heated at 300 °C overnight.
The mass of precipitate was weighed when the crucible is cooled. The percentage of ferum in the
given solution was calculated.
Data
Weight of empty crucible 55.5340 g
Weight of crucible + precipitate 55.5662 g
Weight of precipitate 0.0322 g

Results and Discussion

Mass Fe O
No. of mol Fe2 O3 in sample = Molar mass2Fe3 O
2 3

0.0322 g
=
159.70 g/mol

= 2.0163 × 10-4 mol

2Fe3+ + 3O2- → Fe2 O3

From equation,

1 mol Fe2 O3 ≡ 2 mol Fe3+

2.0163 × 10-4 mol Fe2 O3 ≡ 4.0326 × 10-4 mol Fe3+

Fe2+ → Fe3+ + e-

From the equation,

1 mol Fe3+ ≡ 1 mol Fe2+

4.0326 × 10-4 mol Fe3+ ≡ 4.0326 × 10-4 mol Fe2+

Mass of Fe2+ = No. of mol × Molar mass

= 4.0326 × 10-4 mol × 55.85 g/mol

= 0.0225 g

Mass Fe
Percentage Fe in Fe solution = V of Fe
× 100

0.0225 g
= 25.0 mL × 100

= 0.09%
 From the equation above, Iron (II) ion was oxidised to form Iron (III) ion to form the precipitate. The
colour formed usually was dark-brown colour when it reacts with NH4 OH. NH4 OH act as an
indicator to distinguish the colour so that the presence is much visible. In the experiment, the mass
of precipitate obtained is 0.0322 g and the mass of Fe2+ in sample is 0.0225 g. From that mass, the
exact percentage of fe in fe solution can be determined. From this calculation, we have calculated
the percentage of ferum in a ferum solution by using the mass of Fe. Hence, the percentage of ferum
in a ferum solution is 0.09%.

In this experiment, the steps was taken precautiously in order to have precise and accurate results.
For example, the addition of NH4 OH must be carried out in the fume cupboard in order to prevent
the smell of the compound to be distributed in the laboratory room. At this point, the steps in the
precipitation reaction was taken chronologically, that is the steps were followed strictly in a
gravimetric analysis to get the resulting analysis correctly and to minimize the desirable outcomes of
the analysis.

Conclusion
In the end of the experiment, we had obtain accurately the weight of the precipitate and the
percentage yield by using a gravimetric filtration (Gravimetric Analysis). The weight of the
precipitate obtained in the sample solution is 0.0322 g. Therefore, the percentage of Ferum in a
Ferum solution is 0.09%.

References
Ferum. (n.d.).Ferum. Retrived on December 31, 2022, from
https://docs.ferum.xyz/introduction/overview

Filtration Solution for Gravimetric Analysis. (n.d.). Merckmilipore.

https://www.merckmillipore.com/MY/en/life-science-research/chromatography-sample-
preparation/filtration-methods/general-
filtration/gravimetric/rxmb.qB.9gEAAAFBj0FlvzJY,nav?ReferrerURL=https%3A%2F%2Fuk.sea
rch.yahoo.com%2F&bd=1

Gravimetric Analysis: Precipitate Filtration. (2017, January 19). 911Metallurgist.

https://www.911metallurgist.com/blog/gravimetric-analysis-precipitate-filtration