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Aim:

To prepare the pure samples of crystals of Potassium Ferric Oxalate from oxalic acid dihydrate,
potassium monohydrate and ferric chloride.

Theory:
Potassium ferric oxalate is prepared when freshly prepared ferric hydroxide is dissolved in a
solution of oxalic acid, a yellow precipitate of ferrous oxalate will be formed. It is further treated
with potassium oxalate monohydrate, and a green precipitate of Potassium Ferric Oxalate is
formed. Potassium ferric oxalate is a complex compound with the formula K3[Fe(C2O4)3].3H2O.
The chemical reactions are given below.

FeCl3 + 3KOH → Fe(OH)3 + 3KCl


2Fe(OH)3 + 3(COOH)2.2H2O → Fe2(C2O4)3 + 12H2O
Fe2(C2O4)3 + 3(COOK)2.H2O → 2K3[Fe(C2O4)3].3H2O
(Potassium Ferric Oxalate)

Oxalic acid is added in excess so that ferric hydroxide dissolves and the soluble complex is formed.
Alcohol is added to the solution to precipitate the complex iron salt as it is less soluble in alcohol
than water.
Materials Required:
Oxalic acid hydrate, Ferric chloride, Potassium oxalate, Potassium hydroxide, Beaker, Conical flask,
Tripod stand, Glass rod, Wire gauze, Filter paper, China dish, Funnel
(DRAW ON LEFT SIDE OF WHITE PAGE )

1. Ferric oxalate solution – 1. Potassium Ferric


Fe2(C2O4)3 Oxalate –
K3[Fe(C2O4)3].3H2O
Procedure:
1. In a beaker dissolve 3.5 g of freshly prepared ferric chloride in 10 ml of water.
2. Take another beaker and dissolve 4 g of potassium hydroxide in 50ml of water.
3. Add the potassium hydroxide solution slowly to the ferric chloride solution with constant
stirring. A brown colour ferric hydroxide precipitate is formed
4. Filter the precipitate of ferric hydroxide through the funnel and wash the precipitate with
hot water.
5. In another beaker take 4 g of oxalic acid and 5.5 g of potassium oxalate. Add 100 ml water
and stir well to get a clear solution of potassium oxalate.
6. Add the freshly prepared ferric hydroxide precipitate to potassium oxalate solution gradually
with constant stirring so that precipitate dissolves completely, and the green colour solution
is formed.
7. Filter the solution in order to remove any insoluble impurities.
8. Transfer the green-coloured solution to a china dish and concentrate the solution till
the crystallisation point is achieved.
9. Place the china dish in cold water and allow cooling for an hour.
10.Green crystals of potassium ferric oxalate are formed. Remove the crystals from the mother
liquor.
11.Wash the crystals with ethyl alcohol and dry them between the folds of filter paper.
12.Weigh the crystals in order to know the yield.

Observations:
Colour of the crystals Green colour

Shape of the crystals Octahedral

Melting point 230 oC

Expected yield 10 gm

Results :
The yield of Potassium ferric oxalate is :-9.3gm.

Precautions:
1. Do not concentrate the solution too much.
2. Do not disturb the solution during crystallisation in order to get big crystals.
3. While washing the crystals, wash them with hot water in order to dissolve unwanted salt.

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