FE 211

ANALYTICAL CHEMISTRY

EXPERIMENT-2

ANALYSIS OF IRON IN A SOLUBLE

Uğur ASİT
PURPOSE:

In this experiment we are going to determine iron yield in an aqueous

solution by using gravimetric method. But this time we will treat analyte more
complexly.

THEORY:

Gravimetric method is one of the three subgroups of quantitative analytical

method. It is based on measuring the weight of a known substance which is related
to the analyte and, by using the relation, determining the quantity.
Gravimetric analyses divides into three subgroups; precipitation, volatilization,
electro deposition. In this experiment we are going to use precipitation method.
As we all know solubility varies for all compounds. There are such compounds
that nearly insoluble. Precipitation method is based on this principle that precipitating
a soluble analyte as insoluble compound of it and weighing the precipitation.
We will separate iron crystalline precipitate by filtering and wash it. After
drying and ignition we’ll weigh the pure iron.

MATERIALS:

 Diluted ammonium hydroxide solution (Dilution 1 to 3).

 Filter paper pulp.
 Nitric acid solution.
 Methyl orange indicator (0.02 g/100 ml).
 Silver nitrate solution (5 g/100 ml).
 NH4NO3 solution (1g/100 ml).
 Crucible.
 Flask
 Distilled water.

PROCEDURE:

 We took 5 ml of sample solution.

 This solution was diluted to 250 ml with water.
 It was started to heat solution.
 Filter paper pulp was added to the solution and stirred.
 Three drops of nitric acid were added.
 It was went on heating till boiling
 Three drops of methyl orange was added and solution titrated with ammonium
hydroxide.
 Solution cooled and rested to settle till clear supernatant was observed.
 Precipitation was filtered gently and washed with NH4NO3 till used washing
solution passed the turbidity test (Turbidity test was done with adding a few
drops of AgNO3)
 All content was taken to weighed porcelain crucible and paper was chared off
and ignited at 800 oC.
 Results were reported.
DATA:

Weight of crucible and solid = 12,3487 g

Weight of crucible = 12,2590 g

Weight of solid = 0,0897 g

CALCULATION:

1 lt 60 g Fe 1 mole Fe
Fe in sample : 5 ml * 1000 ml
* 1 lt
* 55.847 g Fe

= 0.0053 mole Fe

1 mole Fe2O3
Found Fe : 0.0897 g Fe2O3 * 159.9622 g Fe2O3

2 mole Fe
1 mole Fe2O3 = 0.0011 mole Fe

0.0011 mole Fe *100 = 20,75 %

Percent Yield:
0.0053 mole Fe

DISCUSSION:

In this experiment we became more familiar to gravimetric analysis. But this time
we followed a more complex procedure in order to adjust sample for precipitation
reaction. We treated sample with nitric acid for all Fe ions to turn into +3 form.
For precipitation solution had to be alkaline medium so we tested the medium
with an indicator. We added filter paper pulps because our precipitation was a little
jelly like and could clog the pours of filtration paper.
As we know Fe is mostly found in nature as mineral forms and it is a good
example for other B group metals that is found in the nature. That is why such
analysis is very important in food sector.
To talk about our experiment a personal mistake occured during experiment that
is why I expect a positive error in results. But experiment can said to successful.