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ABSTRACT

In this experiment, we use a gravimetric analysis method to determine the concentration


Fe in Ferum solution. An analytical chemistry technique called gravimetric analysis uses the mass
of a solid to estimate the amount of an analyte. Example: The solids collected after a known
amount of water has been filtered are weighed. Measuring the solids suspended in the water
sample. Firstly, we need to prepare precipitation from Fe solution. After we got the precipitate, we
need to filter the precipitate and washed the precipitate with warm 1% NH4NO3 solution and
distilled water. Then, put the precipitate into warm crucible and it heated at 600 degrees overnight.
Lastly, weighing the precipitate with the crucible and filled the precipitate into plastic wrap.
INTRODUCTION
According to its definition, gravimetric analysis is based on mass measurements that can
be divided into two categories. These gravimetric analyses are of the sorts of precipitation and
volatilization. By using the precipitation method of gravimetric analysis, a substance can be
quantitatively determined by isolating an ion in solution through a precipitation reaction, filtering,
washing the precipitate free of impurities, converting the precipitate into a product with a known
composition, weighing the precipitate, and then calculating its mass by difference. The amount of
the initial ion can be calculated from the mass and known composition of the precipitate.
In this experiment, the amount of Fe in a certain solution will be found. Iron oxide hydrates,
Fe2O3.XH2O, are precipitated after Fe(II) is oxidised to Fe(III). Fe2O3 precipitate was filtered,
washed, and dried to create ferric oxide. The required substance needs to be totally precipitated
in order to make a valid determination. The precipitate has such a poor solubility in most
determinations that the losses from dissolution are insignificant. The additional Fe3+ that is
supplied reduces the solubility of Fe2O3 even more, tipping the equilibrium to the right. The
product's weighted form should have a known composition. Fe2O3 is a stable chemical, hence it
is possible to compute the mass of Fe in the solution.
OBJECTIVE
The aim for this experiment is to determine the percentage of Ferum in a Ferum solution.
PROCEDURE
A. Preparing a Crucible.
1. We cleaned the crucible.
2. Then, we heated the crucible using a furnace for 10 minutes.
3. The crucible was cooled in a desiccator and lastly, weighed the crucible.

B. Precipitation.
1. The ferum solution was pipetted 25.0mL into 400mL beaker.
2. 25mL of distilled water was added and the beaker was covered with watch glass.
3. Then, ferum solution was heated until boiling.
4. After that, 1mL of concentrated HNO3 was added by dropwisely into the solution.
5. Continue heating the solution until it turns clear and distilled water was added to
200mL for dilute the solution.
6. Heated the solution until boiling and we transferred the beaker into fume cupboard to
added 1:1 NH4OH into solution slowly and stirring until we got the excess.
C. Filtering and Washing the Precipitate.
1. Precipitate was filtered by decantation using filter paper no. 41 without stirring the
solution.
2. Precipitate was washed with 30mL of warm 1% NH4NO3 solutions.
3. Solution was poured into the filter funnel leaving behind most of the precipitate and
repeated it another two times.
4. All the precipitate quantitatively was transferred into the funnel.
5. Then, the precipitate was washed with warm distilled water and test the filtrate for
chloride with acidic silver nitrate solution.

D. Drying and Weighing the Precipitate.


1. The filter paper containing all the precipitate was transferred into the crucible that had
prepared earlier.
2. Crucible containing the precipitate with filter paper was placed into a muffle furnace.
3. Precipitate was heated at 600°C overnight.
4. After crucible was cooled, the mass of precipitate with crucible was weighed.
5. Then, the precipitate was poured into plastic wrap, fold and staple the plastic wrap.
6. The precipitate was submited together with the report.

RESULT
Weight of empty crucible = 70.0808 g
Weight of crucible +
precipitate
1 70.2340 g
2 70.2340 g
3 70.2341 g

Average weight of crucible + precipitate = 70.2340 g


Weight of precipitate, g = 0.1532 g
CALCULATION

2Fe3+ + 3/2O2 Fe2O3

2 mol of Fe3+ : 1 mol of Fe2O3


0.1532 𝑔
2 mol of Fe3+ = 159.7 𝑔/𝑚𝑜𝑙

0.001 𝑚𝑜𝑙
Mol of Fe3+ =
2

Mol of Fe3+ = 0.0005 mol


Mass of Fe3+ = 0.0005 mol x 55.85 g/mol
= 0.028 g
0.0279 𝑔
% (W/V) = 25𝑚𝐿
x 100

= 0.001 %
Thus, the amount of Fe in the sample if 0.001%.

DISCUSSION
In this experiment, the analyte's pH was controlled by the addition of NH4OH, which also
caused a precipitate that could be measured as soon as it had dried completely. The analyte is a
solution of ferum. The study' underlying tenet is that a pure compound's ion mass can be
established and utilised to calculate the mass percent of the same ion in a specific amount of an
impure substance.
The proportion of ferum in a ferum solution has been calculated using the equation used
in the calculation above. The mass of Fe3+ in the solution, which is 0.0279g, is determined using
stoichiometry. The precipitate formed in this experiment weighs 0.1532g and is composed of
Fe2O3. While the ferum content of the ferum solution is estimated to be 0.001%. This
demonstrates that the ferum solution is actually a ferum chloride solution rather than being pure
ferum. The percentage indicates that there is just a small quantity of ferum present in the solution,
with the remainder most likely being chloride or other contaminants.
When handling NH4OH, take care by always using gloves, a mask, goggles, and a lab
coat to avoid any potential hazards from the NH4OH's indecent odour and breathing difficulties.
There could be mistakes made throughout the experiment, including introducing more HNO3
drops than the lab manual recommends. The outcome may also be impacted by this.
CONCLUSION
The experiment's goal has, therefore, been successfully attained. In a ferum solution,
ferum makes up 0.001% of the mixture.
REFERENCE
1. gravimetric analysis - Google Zoeken. (n.d.).

https://www.google.com/search?q=gravimetric+analysis

2. Wikipedia contributors. (2022, September 25). Gravimetric analysis. Wikipedia.

https://en.wikipedia.org/wiki/Gravimetric_analysis

3. The Editors of Encyclopaedia Britannica. (2022, October 26). Gravimetric analysis |

Definition, Steps, Types, & Facts. Encyclopedia Britannica.

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

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