Introduction

Ferrous ammonium sulfate was dissolved in a slightly acid solution, excess oxalic acid , H2C2O4
is added, and the balance chemical reaction below show the reaction take place in the
experiment:
Fe(NH4)2(SO4)2.6H2O + H2C2O4 FeC2O4(s) + H2SO4 + (NH4)2 + 6H2O(l)
FeC2O4(s) is a finely divided precipitate and tends to colloidal. When the solution was heated it
may causes the solution to coagulate and the facilities separating the precipitate from the
solution. FeC2O4(s) precipitate was added with potassium oxalate which produces a slightly basic
solution for the oxidation of the ferrous ion to the ferric ion to the by hydrogen peroxide, H2O2.
The following reaction takes place:
-

H2O + HO + 2Fe 2Fe + 3OH2

2+

3+

The OH- ion concentration of the solution is high enough so that some Fe3+ reacts with the OH- to
form ferric hydroxide that is brown precipitate as follows:
Fe + 3OH- Fe(OH) (s)
3+

With addition of more H2C2O4, the Fe(OH)3 dissolves and the soluble complex
K3[Fe(C2O4)3].3H2O in form ferric hydroxide (brown precipitate) as follows:
3K2C2O4 + 2Fe(OH)3(s) + 3H2C2O4 2K3[Fe(C2O4)3]. 3H2O + 3H2O
Ethanol is added to the solution to cause the complex iron salt to precipitate.
Objective
The purpose of this experiment is to synthesize potassium tris(oxalate) ferrate(III) trihydrate
K3[Fe(C2O4)3].3H2O.
Apparatus and chemicals
Ferrous ammonium sulfate
Distilled water
Oxalic acid dehydrate
Hot plate
Potassium oxalate monohydrate
Beaker
Spatula
Suction filtration

Procedure
Procedure A
1. 5.00g of ferrous ammonium sulfate in 20ml of water containing 1ml of dilute sulfuric
acid in beaker.
2. 2.5g of oxalic acid dehydrate in 25ml of water were added.
3. Slowly heated the mixture to boiling and allow the yellow precipitate settle. Decant the
supernatant.
4. 15ml of hot water were added to yellow precipitate, stir and decant the supernatant.
5. 15ml hot water was added to precipitate.
6. 3.50g solid potassium oxalate monohydrate was added and heated to 40oC.
7. Immediately added 10ml of 6% H2O2 dropwise and stirred continuously at temperature
40oC
8. Periodically check the temperature of solution at least 40oC during added of H2O2
9. Heated to boil and 2.00g of oxalic acid dehydrate was added in 30ml of water.
10. 20ml was added initially then added more solution little by little until dissolves all brown
precipitate.
11. The clear solution was boiled, filter bunchier funnel with well fitting paper and 30ml
95% ethanol was added slowly.
12. The crystals heated to redissolve and leaved to crystalize
Procedure B
1. The crystals obtained using suction filtration.
2. The crystal washed twice with a cooled 1:1 ethanol / water mixture and finally with
cooled acetone.
3. Stored in beaker and wrapped with vial.