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OBJECTIVES
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 dropwisely. 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.
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.
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
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
16.2% besides, the Fe that contains 5.7952g of Fe2O3 is 4.0536g.
In this experiment, the steps was taken precautiously. For example, 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. 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 16.2%.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