EXPERIMENT 3

Determination of the Percentage of Ligands in K3[Fe(C2O4)3].3H2O

Objectives:
1. To standardize the potassium permanganate solution.
2. To determine the percentage of ligands in K3[Fe(C2O4)3].3H2O.

Introduction
Standardization of potassium permanganate (KMnO4) solution is carried out by
titration against a standard solution of oxalic acid. Oxalic acid is a good primary
standard because the compound is available in solid form, as H 2C2O4.2H2O, which
can be prepared to a very high degree of purity and is not hygroscopic nor efflorescent.

The reaction is as follows:

Reduction: 2(MnO4− + 5e− + 8H+ → Mn2+ + 4H2O)

Oxidation: 5(H2C2O4 → 2CO2 + 2e− + 2H+)

Overall reaction: 2MnO4− (aq) + 6H+ (aq) + 5H2C2O4 (aq) → 2Mn2+ (aq) + 8H2O (l)
+ 10CO2 (g)

The following points about this reaction should be noted:

1. The reaction occurs only in acidic solutions. Acidification is achieved by the

addition of sulfuric acid.

2. The reaction rate is normally slow, however, in this experiment, (i) is increased by
warming the contents of the conical flask, (ii) because the reaction is catalysed by
the presence of manganese(II) ion, which is a product of the reaction.

No indicators are necessary in this titration. As the permanganate solution is added to

the oxalic acid solution, the purple MnO4− ion is reduced to the colourless Mn2+ ion.
When the addition of one drop of permanganate solution to the conical flask produces
a permanent pink colour, this indicates that there is no remaining oxalic acid capable
of reducing the MnO4− ion to Mn2+ ion, and therefore, the end point has been reached.

Safety precautions
All chemicals are toxic. The organic solvents are highly flammable and can be irritating
to body tissues and respiratory tract. Acids are corrosive. Work with care and wear
safety goggles. Wash hands thoroughly with soap and water before leaving the
laboratory.
Apparatus
Part A
Balance
Beakers (two 100 mL, one 250 mL)
Volumetric flask (250 mL)
Storage bottle (250 mL)
Pipette (20 mL)
Pipette filler
Burette and stand
Filter funnel
Conical flask (250 mL)
Thermometer

Part B
Balance
Volumetric flask (250 mL)
Storage bottle (approximately 250 mL)
Pipette (20 mL)
Pipette filler
Burette and stand
Filter funnel
Conical flask (250 mL)
Thermometer

Chemicals
Part A
Potassium permanganate solution, KMnO4 0.02 M (300 mL)
Oxalic acid, H2C2O4.2H2O, 0.05 M (250 mL)
Sulphuric acid, H2SO4, 2 M (250 mL)

Part B
Potassium permanganate solution, KMnO4 that has been standardised in Part A (300
mL)
Sulphuric acid, H2SO4 1 M (250 mL)
Complex compound, K3[Fe(C2O4)3].3H2O

Procedure

A. Standardisation of Potassium Permanganate Solution

1. Fill a burette with the KMnO4 solution to be standardised.

2. Pipette 20 mL of the standard oxalic acid solution into a 250 mL conical flask and
add about 20 mL of 2 M H2SO4.
3. Warm the conical flask to about 80°C and titrate the permanganate solution
against the oxalic acid solution. Add the KMnO4 solution slowly or manganese(IV)
oxide (a brown solid) may form instead of manganese(II) ion. The end point is
reached when the addition of one drop permanganate solution produces a
permanent pink colour. Record your results in a table shown below.

4. Repeat the titration until consistent results are obtained.

Data and Observation:

Rough Accurate titrations

estimation 1 2
Final burette reading (mL)

Initial burette reading (mL)

Vol. of KMnO4 used (mL)

B. Determination of the Percentage of Ligands in K3[Fe(C2O4)3].3H2O

1. Weigh out 0.20 g of the coordination compound that was previously prepared.

2. Boil the sample with 50 mL of 1 M sulphuric acid in a conical flask.

3. Allow the solution to cool to 60oC and titrate slowly with the KMnO4 solution
provided (KMnO4 that is standardised in Part A).

4. The end point is reached when the addition of one drop of permanganate solution
produces a permanent pink colour. Record your results in a table shown below.

5. Repeat the titration until consistent results are obtained.

Data and Observation:

Rough Accurate titrations

estimation 1 2
Final burette reading (mL)

Initial burette reading (mL)

Vol. of KMnO4 used (mL)

Questions (to be included in your lab report)

Part A
1. From the average volume of KMnO4 solution used, calculate the concentration of
the solution.

2. Why is it necessary to heat the oxalic acid solution?

3. In this experiment oxalic acid is used as a reducing agent. Could oxalic acid be
used as a primary standard to standardise a solution of a base, such as sodium
hydroxide? Explain your answer.

Part B
1. Given that MnO4− ion is being reduced to Mn2+ ion, and C2O42− ion is being
oxidised to CO2, write a balanced redox equation for the above titration. Use the
equation to calculate the concentration of the oxalate ions in the coordination
compound.

2. Calculate the percentage by weight of oxalate ions in the complex. Compare this
with the theoretical value and thus obtain the percentage purity of the complex.