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ABSTRACT

The experiment Determination of Ferum In a Ferum Solution By Gravimetric Analysis is conducted in


a Ferum solution. There are four parts in this experiment which are preparing a crucible, precipitation
reaction, filtering and washing the precipitate and drying and weighing the precipitate. For Part A,
which is preparing a crucible, a crucible was weighed together with its lid and was heated it in a furnace
for 10minutes. Next, it was cooled in dessicator and was weighed accurately. For Part B, which is
precipitation reaction, it is done by pipetting 25.0mL of Fe solution into 400mL beaker and add 25mL
distilled water and cover with watch glass followed with boiling process. Next,1mL of concentrated
HNO3 was added drop wisely. It was continued heating until the solution becomes clear. Next, the
solution is diluted to 200mL with distilled water and the solution was boiled again. Cautiously, transfer
the beaker to the fume cupboard and add 1:1 NH4OH into the solution slowly and with stirring, until
it is in excess. It would noticed that when there is no more formation of the precipitate and also when
the steam odour is smelled. From the experiment that is carried out, we can obtain the weight of
precipitate in the determination of Fe in a Ferum solution. The weight of precipitate obtained in the
experiment is 0.0209g. Besides, the mass of Fe that contains of of Fe2O3obtained is 0.6994g and the
weight percent,%(w/v)of the analyte in the sample solution obtained in the experiment is 0.08%.

OBJECTIVES

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

INTRODUCTION

In this technique, the analyte is converted to an insoluble form which can then be washed, dried, and
weighed in order to determine the concentration of the analyte in the original solution. Gravimetry is
applied to samples where a good precipitating agent is available. The precipitate should be
quantitative, easily washed and filtered and is of in suitable quantity for accurate weighing. Therefore,
gravimetry is regarded as a macro analytical technique. However, it is considered, when appropriately
done, one of the most accurate analytical techniques. Also, Gravimetry is one of a few analytical
methods that do not require standard solutions as the weight of precipitate is the only important
parameter in analyte determination.

The concentration of Fe in a given solution will be determined in this experiment. Fe(II) is oxidised to
Fe(III) and then precipitated as ferric oxide hydrates,Fe2O3.XH2O.To produce ferric
oxide,Fe2O3,filtered,washed and dried the precipitate. We can calculate the mass of Fe in the solution
since Fe2O3 is a stable compound. There is a long waiting period in this experiment that we need to
manage time well. We should know what to do during the waiting period if we have rea and planned
work well.
PROCEDURE

A.Preparing a Crucible

A crucible together was cleaned with its lid and it was heated in a furnace for 10 minutes. It was
cooled in a desiccators and was weighed accurately.

B.Precipitation

25.0mL ferum solution was pipette into a 400mL beaker,25mL distilled water was added and was
covered with watch glass. The solution was heated to boiling, then 1mL concentrated HNO3 was
added drop wisely. Heating was continued until the solution becomes clear. The solution was diluted
to 200mL with distilled water and the solution was boiled again. The beaker was transferred
cautiously to the fume cupboard and 1:1 NH4OH was added into the solution slowly and with
stirring, until it is in excess. There no more formation of the precipitate was noticed and also when
the steam odour was smelled.

C.Filtering and Washing the Percipitate

The precipitate was filtered by decantation using filter paper no. 41 without stirring the solution to
ensure that most of the precipitate will be left behind in the beaker. Then the precipitate was
washed with 30mL warm 1% NH4NO3solutions.The solution was poured into the filter funnel leaving
behind most of the precipitate. This was repeated for another two times and finally all the
precipitate was transferred quantitatively into the funnel. This could be done with the help of a
rubber policeman and a wash bottle. Finally, the precipitate was washed in the funnel using warm
distilled water and the filtrate was tested for chloride with acidic silver nitrate solution. The test
should turned out positive, the washing process was repeated with more distilled water.

D. Drying and Weighing the Precipitate

The filter paper containing all the precipitate was transferred into the crucible that have prepared
earlier on. The crucible was heated using a Bunsen burner with a small flame at the beginning until
the paper has burned. The flame was increased and heating was continued for another 20 minutes.
The heating process was repeated until a constant mass is obtained. Alternatively, if time did not
permitted, the crucible containing the precipitate and filter paper were placed into a muffle furnace.
The position of the crucible was recorded on the piece of paper at the furnace. The precipitate will
be heated at 600℃ overnight. Once the crucible is cooled, the mass of the crucible and precipitate
were weighed. The precipitate was poured into a plastic wrap, the plastic wrap was folded and
stapled at the top so as to contain the precipitate inside the wrap. The product was submitted
together with the report. The precipitate was ensured to be well contained in the plastic and did not
leak out from the plastic wrap.
RESULTS

Weight of empty crucible = 50.4028 g

Weight of crucible + precipitate = 50.4327 g

Weight of precipitate , g = 0.0299 g

CALCULATION

Gravimetric factor = 2 x Fe = 2 x 55.85 g/mol = 0.6994

Fe₂O₃ 2(55.85) + 3(16)

Weight of analyte = 0.0299 g x 0.6994 = 0.0209 g

Percentage of Fe = 0.0209 g x 100% = 0.08%

25mL

DISCUSSION

The experiment which is Determination of Fe in a Ferum Solution by gravimetric analysis is conducted


in the experiment is to determine the percentage of Ferum in a Ferum solution. In this experiment,
four parts of the experiment were conducted which are the preparation of a crucible ,precipitation
reaction, filtering and washing the precipitate and drying and weighing the precipitate. In this
experiment, the law was used, which is the law of conservation of mass. According to the law, the law
of conservation of mass states that the matter can be interchanged from one form to another form.
According to these law, the mixture can be separated and the pure substances can be decomposed,
but the total amount of mass of the substance remained constant. In this experiment, the
determination of Fe in the unknown Ferum Solution is carried out by using gravimetric.

In this experiment, the process of retrieving of Fe in a Ferum solution usually consumes much time
and can also lead to certain random error such as the personal error and the instrument error to be
occurred.

From the equation, Iron (II) ion was oxidised to form Iron (III) ion to form the precipitate. The colour
formed usually dark-brown colour when it reacts with NH4OH. The function of adding NH4OH is to
distinguish the colour so that the presence is much visible. In the experiment, the mass of precipitate
obtained is 0.0299 g and the weight percent, %(w/v) of the analyte obtained in the experiment is
0.08% besides, the Fe that contains of Fe2O3 is 0.6994g.

In this experiment, the steps was taken precautiously to get the best results .The addition of NH4OH
must be carried out in the fume cupboard in order to prevent the smell of the compound to be
distributed in the laboratory room. Make sure you stop the addition NH₄OH as you swirl it when theres
no more precipitate formed. At this point, the steps in the precipitation reaction was taken
chronologically, that is the steps were followed strictly in a gravimetric analysis in order to get the
resulting analysis and to minimize the desirable outcome of the analysis.
CONCLUSION

In the nutshell , we can obtain accurately the weight of the precipitate and the percent weight,%(w/v)
of the precipitate by using a gravimetric filtration (Gravimetric Analysis).In the experiment, the weight
of the precipitate obtained is in the sample solution is 0.0209 g. Therefore, the percentage of Ferum
in a Ferum solution is determined.

REFERENCES

1. Zuraidah Abdullah Munir, Zaini Hamzah, Sabarina Md Yunus (2014), Analytical Chemistry
Laboratory manual, published by UITM PRESS.
2. Christian, G.D. Analytical chemistry (2003),6th Ed.US:Wiley International Edition.
3. Hall, J, F experiment Chemistry ( 1993 ),3rd edition. Prentice Hall, USA.