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Aim: Volumetric estimation of nitrite in the given solution of sodium nitrite using KMnO4.
Chemicals: Potassium permanganate, sulphuric acid, sodium oxalate, sodium nitrite.
Apparatus: Standard volumetric flask, pipette, burette, conical flask, beakers, funnel and glass rod.
Theory: The aqueous solution of KMnO4 needs to be standardized using sodium oxalate. Nitrite is
oxidized using KMnO4 in an acidic medium. In the estimation of nitrite, the acidified KMnO4 is taken
in a beaker and titrated against sodium nitrite solution, as H2SO4 reacts with nitrite to give nitrous acid
which decomposes to nitrous oxide and water.
Reactions:
2KMnO4 + 5H2C2O4 + 3H2SO4  2MnSO4 + K2SO4 + 10CO2 + 8H2O
5NaNO2 + 2KMnO4 + 3H2SO4 5NaNO3 + 2MnSO4 + K2SO4 + 3H2O
Procedure:
i) Preparation of 0.01N KMnO4 (500 mL) [molecular weight check on the chemical container], calculate
ii) Preparation of 2N H2SO4 (250 mL) [Laboratory normality 36 N],calculate
iii) Preparation of 0.01N Na2C2O4 (500mL) [molecular weight check on the chemical container], calculate
vi) Standardization of KMnO4
Rinse the clean burette with a minimum quantity of KMnO4 and fill it appropriately. Pipette out 10 mL
of 0.01 N sodium oxalate solution in a clean conical flask. Add about 20 mL of 2N H2SO4. Heat the
solution in the flask to about 60 °C. Titrate it against KMnO4, until light pink color permanently
develops in the flask. Repeat the titration to get constant readings.
v) Estimation of nitrite.
Rinse the clean burette with a minimum quantity of sodium nitrite solution and fill it appropriately.
Pipette out 10 mL of given KMnO4 solution in a clean beaker and add 40 mL of 2N H2SO4. Warm the
solution from the beaker (40 °C). Dip the tip of the burette in solution in the beaker. Titrate the solution
from the beaker against the nitrite solution, until the pink color of KmNO4 disappears. Repeat the
titration to get the constant readings.
Results:
i) The amount of nitrite in 100 mL is ___g.
ii) The amount of sodium nitrite in 100 mL is ___g.
Further reading (available in the library)
1) Experiments in Applied Chemistry, S. Rattan, S. K Kataria and Sons.
2) Vogel’s textbook of quantitative chemical analysis, J. Mendham, R. C. Denney, J. D. Barns, M.
Thomas, B. Sivasankar, Pearson India Education, 6th
Edition.
Questions.
1) Calculate the oxidation state of nitrogen in nitrate and nitrite.
2) Can we use not HCl or HNO3 in redox titrations?
3) Is it possible to quantitatively determine ferric ions by this method?
4) Why the tip of the burette is dipped in the solution?

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Volumetric estimation of nitrite in the given solution of sodium nitrite using KMnO4

  • 1. Aim: Volumetric estimation of nitrite in the given solution of sodium nitrite using KMnO4. Chemicals: Potassium permanganate, sulphuric acid, sodium oxalate, sodium nitrite. Apparatus: Standard volumetric flask, pipette, burette, conical flask, beakers, funnel and glass rod. Theory: The aqueous solution of KMnO4 needs to be standardized using sodium oxalate. Nitrite is oxidized using KMnO4 in an acidic medium. In the estimation of nitrite, the acidified KMnO4 is taken in a beaker and titrated against sodium nitrite solution, as H2SO4 reacts with nitrite to give nitrous acid which decomposes to nitrous oxide and water. Reactions: 2KMnO4 + 5H2C2O4 + 3H2SO4  2MnSO4 + K2SO4 + 10CO2 + 8H2O 5NaNO2 + 2KMnO4 + 3H2SO4 5NaNO3 + 2MnSO4 + K2SO4 + 3H2O Procedure: i) Preparation of 0.01N KMnO4 (500 mL) [molecular weight check on the chemical container], calculate ii) Preparation of 2N H2SO4 (250 mL) [Laboratory normality 36 N],calculate iii) Preparation of 0.01N Na2C2O4 (500mL) [molecular weight check on the chemical container], calculate vi) Standardization of KMnO4 Rinse the clean burette with a minimum quantity of KMnO4 and fill it appropriately. Pipette out 10 mL of 0.01 N sodium oxalate solution in a clean conical flask. Add about 20 mL of 2N H2SO4. Heat the solution in the flask to about 60 °C. Titrate it against KMnO4, until light pink color permanently develops in the flask. Repeat the titration to get constant readings. v) Estimation of nitrite. Rinse the clean burette with a minimum quantity of sodium nitrite solution and fill it appropriately. Pipette out 10 mL of given KMnO4 solution in a clean beaker and add 40 mL of 2N H2SO4. Warm the solution from the beaker (40 °C). Dip the tip of the burette in solution in the beaker. Titrate the solution from the beaker against the nitrite solution, until the pink color of KmNO4 disappears. Repeat the titration to get the constant readings. Results: i) The amount of nitrite in 100 mL is ___g. ii) The amount of sodium nitrite in 100 mL is ___g. Further reading (available in the library) 1) Experiments in Applied Chemistry, S. Rattan, S. K Kataria and Sons. 2) Vogel’s textbook of quantitative chemical analysis, J. Mendham, R. C. Denney, J. D. Barns, M. Thomas, B. Sivasankar, Pearson India Education, 6th Edition. Questions. 1) Calculate the oxidation state of nitrogen in nitrate and nitrite. 2) Can we use not HCl or HNO3 in redox titrations? 3) Is it possible to quantitatively determine ferric ions by this method? 4) Why the tip of the burette is dipped in the solution?