Preparation of Potassium Ferric Oxalate

Potassium Ferric Oxalate crystals is a light green color complex compound prepared from ferric sulfate and barium oxalate in the presence of oxalic acid. This preparation of potassium ferric oxalate is an example of an Oxidation-Reduction reaction.

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, yellow precipitate of ferrous oxalate will be formed. It is further treated with potassium oxalate monohydrate, 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.

Other names – Potassium Trioxalatoferrate (III), Potassium ferrioxalate, Potassium iron(3+) oxalate, Potassium tris(oxalato)ferrate(III)

Materials Required:

  1. Oxalic acid hydrate
  2. Ferric chloride
  3. Potassium oxalate
  4. Potassium hydroxide
  5. Beaker
  6. Conical flask
  7. Tripod stand
  8. Glass rod
  9. Wire gauze
  10. Filter paper
  11. China dish
  12. Funnel

Apparatus Setup:

Preparation of Potassium Ferric Oxalate

  1. Ferric oxalate solution – Fe2(C2O4)3
  2. Potassium Ferric Oxalate – K3[Fe(C2O4)3].3H2O

Procedure:

  1. In a beaker dissolve 3.5g of freshly prepared ferric chloride in 10 ml of water.
  2. Take another beaker and dissolve 4g of potassium hydroxide in 50ml of water.
  3. Add the potassium hydroxide solution slowly to 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 4g of oxalic acid and 5.5g of potassium oxalate. Add 100ml 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 green colour solution is formed.
  7. Filter the solution inorder to remove any insoluble impurities.
  8. Transfer the green coloured solution in a china dish and concentrate the solution till the crystallization point is achieved.
  9. Place the china dish in cold water and allow to cool for an hour.
  10. Green crystals of potassium ferric oxalate is 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

230oC

Expected yield

10 gm

Results and Discussion:

The yield of Potassium ferric oxalate is _______gm.

Precautions:

  1. Do not concentrate the solution too much
  2. Do not disturb the solution during crystallization inorder to get big crystals.
  3. While washing the crystals wash it with hot water in order to dissolve unwanted salt.

Viva Questions:

1. What is the colour of Potassium ferric oxalate and what is its melting point?

The colour of Potassium ferric oxalate is green and its melting point is 230oC.

2. What is meant by equimolar proportions?

Proportion of the substances in the ratio of their molecules 1:1 mole ratio.

3. Define crystallization?

Crystallization is the process through which a solid form is formed, where the atoms or molecules are highly organized into a structure called a crystal.

4. What is called “seeding”?

In some cases crystallization does not occur, if crystal of same substance is added to the saturated solution induce crystallization. This is called seeding.

5. Give the relation between specific conductivity and resistance of a solution?

The relation is,

Specific conductance = Cell constant x (1/Resistance)

Leave a Comment

Your email address will not be published. Required fields are marked *