Experiment. No. 4
OBJECTIVE:
TO STANDARDIZE THE GIVEN POTASSIUM PERMANGANATE SOLUTION BY USING N/10 STANDARD OXALIC ACID SOLUTION AND EXPRESS THE CONCENTRATION IN TERMS OF MOLARITY, GRAM PER LITRE AND PERCENTAGE STRENGTH
APPARATUS REQUIRED
- conical flask
- pipette
- burette
- beaker
- glass tube
CHEMICALS REQUIRED
- Potassium permanganate
- oxalic acid
- sulphuric acid
THEORY
Standardization means the determination of the concentration of an unknown solution with the help of the primary standard solution by finding the endpoint of the reaction. The reaction between the acidified KMnO4 solution and the oxalic acid solution is oxidation-reduction and is said to be a redox reaction. KMnO4 acts as an oxidizing agent and Oxalic acid acts as a reducing agent. The titration between oxidizing and reducing agents is called redox titration. The concentration of unknown KMnO4 solution is determined by titrating it against a certain volume of oxalic acid. At the endpoint, the KMnO4 solution persists in its pink colour. Therefore, potassium permanganate itself acts as self indicator.
Formula unit equation
KMnO4 + 3H2SO4 + 5H2C2O4 → K2SO4 + 2MnSO4 + 8H2O + 10CO2
Ionic equation
In this reaction, H2SO4 acts as an acidifying agent. Here Magnesium is reduced from +7 to +2 oxidation state by gaining 5 electrons. So, the equivalent weight of KMnO4 is calculated by dividing molecular weight by 5.
Eq. wt. = 158/5 = 31.6
PROCEDURE
A clean burette was taken and clamped in a stand in a vertical position. Then the burette was rinsed with KMnO4 solution and filled with it. The pipette was rinsed with standard oxalic acid solution and pipetted out 10 ml of the solution in a clean conical flask. Then, 1 test full of H2SO4 solution was added and heated at about 60-70°C. While hot, it was titrated by adding KMnO4 solution from the burette in a small amount swilling the flask all the while. The pink colour of KMnO4 will go on disappearing. The addition of KMnO4 solution was continued till a last single drop until a light pink colour persisted for a few seconds. This was the endpoint of the titration. The titration was repeated till till concurrent reading was obtained.
OBSERVATION TABLE
S.N. | Vol. of oxalic acid taken (ml) | Burette reading (ml) (KMnO4) | Concurrent reading | ||
Initial | Final | Difference | |||
1. | 10 | 0.0 | 10.5 | 10.5 | |
2. | 10 | 10.5 | 20.6 | 10.1 | 10.1 |
3. | 10 | 20.6 | 30.7 | 10.1 |
CALCULATION
KMnO4 Taken | Oxalic acid taken |
V1 =10.1 ml N1 = ? | V2 =10ml N2 = N/10 |
From Normality equation,
V_{1}N_{1} = V_{2}N_{2}\\ 10.1 \times N_{1} =10 \times (1/10)\\ N_{2} = 0.099 N
Normality = 0.099 N
Molarity = Normality/n = 0.099/5 = 0.0198 M
Gram per litre = Normality x eq. wt. = 0.099 x 31.6 = 3.1284 gm/lit
Percentage strength = (gm/lit)/10 = 3.1284/10 = 0.31284 %(w/v)
RESULT
Hence, the given KMnO4 solution was standardised and it’s concentration was found to be 0.099N
CONCLUSION
Redox titration can be carried out without using an indicator.
PRECAUTIONS
- The burette was not used with a rubber cock.
- The reading was taken coinciding with the upper meniscus of the burette.
- Titration must be carried out in a hot solution.
- A sufficient quantity of dilute sulphuric acid was added to the oxalic acid solution in the titrating flask before titration.
- Care should be taken while sucking oxalic acid so that no solution comes into the mouth as it is poisonous.
- A small quantity of KMnO4 was added at a time and shaken till it was decolourized before adding the next lot.
- At the end of the experiment, the whole apparatus was washed with water. Burette and beaker, which contained KMnO4 solution usually, get a brown stain. Clean these with FeSO4 solution and wash them again with water.