OBJECTIVE

1. To determine the percentage of Ferum in a Ferum Solution

INTRODUCTION
Gravimetric analysis is a method of quantitative chemical analysis in which the constituent
sought is converted into a substance (of a known composition) that can be separated from the
sample and weighed. The steps commonly followed in gravimetric analysis are 1) preparation
of a solution containing a known weight pf a sample, 2) separation of the desired content,3)
weighing the isolated constituent, and 4) computation of the amount of the constituent in the
sample from the observed weight of the isolated substance. For this experiment, the
concentration of Fe was determined in a given solution. Fe (II) is oxidised to Fe (III) and then
precipitated as ferric oxide hydrates, 𝐹𝑒2 𝑂3 ∙ 𝑋𝐻2 𝑂. The precipitate is filtered, washed, and
dried to produce ferric oxide, 𝐹𝑒2 𝑂3 . Since 𝐹𝑒2 𝑂3 is a stable compound, we can calculate
the mass of Fe in the solution.

PROCEDURE
A. PREPARING A CRUCIBLE
1. A crucible with its lid was cleaned and heated in a furnace for 10 minutes. Then the
crucible was cooled down in a desiccator and weighed accurately.

B. PRECIPITATION
1. 25 ml of ferum solution was pipetted into a 400 ml beaker and 2 ml of distilled water
was added and the beaker was covered with watch glass.
2. The solution was heated to boiled and 1 ml of concentrated 𝐻𝑁𝑂3 was added drop
wisely.
3. The heating was continued until the solution becomes clear. The solution was diluted
to 200 ml with distilled water and let boiled again.
4. The beaker was transferred to the fume cupboard and 1:1 𝑁𝐻4 𝑂𝐻 was added to the
solution slowly and with stirring until it in excess.

C. FILTERING AND WASHING THE PRECIPITATE

1. The precipitate was filtered out by decantation using a filter paper no.41 without stirring
the solution to ensure that most of the precipitate will be left behind in the beaker.
2. The precipitate then washed with 30 ml of warm 1% 𝑁𝐻4 𝑁𝑂3 solution. The solution
was poured into the filter funnel leaving behind most of the precipitate. This seps was
repeated 2 times and finally all the precipitate was transferred quantitatively into the
funnel.
3. The precipitate in the funnel was then washed with distilled water and the precipitate
was tested for chloride with acidic silver nitrate solution.
D. DRYING AND WEIGHING THE PRECIPITATION
1. The filter paper containing all the precipitate was transferred into the crucible that have
been weighed. The crucible was heated using a Bunsen burner with a small flame at the
beginning, until all the paper has burned. The flame was increased and continued for
another 20 minutes.
2. The heating process was repeated until a constant mass is obtained.
3. Alternatively if time was not permitted, the crucible containing the precipitate and filter
paper was placed into a muffle furnace. The precipitate will be heated overnight.
4. Once the crucible is cooled, the weight of the mass of crucible and precipitate was
weighted.

RESULT
Weight of empty crucible (g) 69.3955
Weight pf crucible + precipitate (g) 69.5475
Weight of precipitate (g) 0.152

CALCULATION

𝑚𝑎𝑠𝑠 𝑜𝑓 𝐹𝑒2 𝑂3
𝑚𝑜𝑙 𝑜𝑓 𝐹𝑒2 𝑂3 =
𝑚𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 𝑜𝑓 𝐹𝑒2 𝑂3

0.1520
= 2(55.85)+3(16)

= 0.0009518 mol

2𝐹𝑒 3+ + 3𝑂2− → 𝐹𝑒2 𝑂3

From equation:
2 mol of 𝐹𝑒 3+ produce 1 mol of 𝐹𝑒2 𝑂3
X mol of 𝐹𝑒 3+ produce 0.0009518 mol of 𝐹𝑒2 𝑂3
X = 0.0009518 × 2
= 0.0019036 mol

Mol of 𝑭𝒆𝟑+ = 0.0019036 mol

𝐹𝑒 2+ → 𝐹𝑒 3+ + 𝑒 −
From the equation:
1 mol of 𝐹𝑒 2+ produce 1 mol of 𝐹𝑒 3+
0.0019036 mol 𝐹𝑒 2+ produce 1 mol of 𝐹𝑒 3+
Mol of 𝑭𝒆𝟐+ = 0.0019036 mol
Mass of 𝑭𝒆𝟐+ = 𝑚𝑜𝑙 × 𝑚𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠
= 0.0019036 × 55.85
= 0.106 g
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒
% weight / volume = 𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 × 100
0.106 𝑔
= × 100
25 𝑚𝑙

= 0.424 %
DISSCUSSION
This experiment was conducted to determine the percentage of ferum in ferum solution by
gravimetric analysis techniques. Start from preparing the crucible, to preparation of precipitate
reaction ( Fe(II) oxidised to Fe(III)) to produce ferum oxide hydrates which is the precipitate .
filtering and washing the precipitate and dry and weighting the obtained precipitate. Based on
the equation 𝐹𝑒 2+ → 𝐹𝑒 3+ + 𝑒 − , Fe(II) was oxidised to Fe(III) and Fe(III) react with oxygen
ion to form ferum oxide hydrates which is the precipitate. The colour of the precipitate obtain
in the solution was turned out to be intense brown coloured. The precipitate was then been
filtered out and washed with 𝑁𝐻4 𝑁𝑂3 and distilled water. Then the precipitate was dried in
the furnace for about one night and the mass was weighed. The mass 𝐹𝑒2 𝑂3 of obtained from
all the process above was 0.152 g. with the amount of mass obtained the mol of 𝐹𝑒2 𝑂3 was
calculated and the result was 0.0009158 mol. By stoichiometry,
3+ 2− 3+
2𝐹𝑒 + 3𝑂 → 𝐹𝑒2 𝑂3 , we know that 2 mol of 𝐹𝑒 produce 1 mol of 𝐹𝑒2 𝑂3 , and from
there, we can know that the mol of 𝐹𝑒 3+ is 0.0019036 mol. By using the second equation which
is 𝐹𝑒 2+ → 𝐹𝑒 3+ + 𝑒 − , 1 mol of 𝐹𝑒 2+ produce 1 mol of 𝐹𝑒 3+ and the number of mol for
𝐹𝑒 2+ 𝑖𝑠 0.0019036 mol. With the value of the number of mol of Fe(II) the mass of Fe(II) was
calculated to be 0.106 g and the %(w/v) is 0.424%.

CONCLUSION
In can be conclude that the obtained mass of the precipitate 𝐹𝑒2 𝑂3 is 0.152 g and the mass of
Fe (II) was 0.106 g with the %(w/v) 0.424 %

REFERENCES
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analysis/#:~:text=What%20is%20Gravimetric%20Analysis%3F,the%20collected%20

solids%20are%20weighed.
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Definition, Steps, Types, & Facts. Encyclopedia Britannica.

https://www.britannica.com/science/gravimetric-analysis

3. PubChem. (n.d.). Iron(III) oxide. PubChem.

https://pubchem.ncbi.nlm.nih.gov/compound/Iron_III_-oxide