TITRATION INVOLVING AQUEOUS POTASSIUM PERMANGANATE (PERMANGANOMETRY)

Potassium permanganate is a powerful oxidizing agent in the presence of an acid .In acidic medium it oxidizes oxalic acid to carbon dioxide; metal oxalate to metal salt and carbon dioxide, ferrous salts to ferric salts and so on. In acid solution the reaction can be represented by the following equation: MnO4- + 8H+ + 5e2MnO4- + 10Cl- + 16H+ Mn2+ + 4H2O 2Mn2+ + 5Cl2 + 8H2O

Sulphuric acid is the most suitable acid .With hydrochloric acid, the reaction

may take place and some permanganate may be consumed in the formation of chlorine (side reaction). Therefore, HCl should not be used to acidify KMnO4. It is difficult to obtain potassium permanganate perfectly pure and completely free from manganese dioxide (MnO2). Moreover, ordinary distilled water is likely to contain reducing substances (traces of organic matter etc.) which will react with the potassium permanganate to form MnO2, which in turn, catalyses the auto decomposition of the permanganate solution on standing. Due to these reasons potassium permanganate solution is not primary standard, that is, KMnO4 solution of desired concentration cannot be prepared simply by dissolving calculated amount of potassium permanganate crystals. Therefore, potassium permanganate solution is standardized just before it is used to titrate other solutions. Potassium permanganate solution may be standardized using standard sodium oxalate or oxalic acid. In acidic medium, oxalic acid reduces MnO4- giving colourless solution. MnO4- + 8H+ + 5e(COOH)2 2MnO4- + 6H+ + 5(COOH) 2 Mn2+ + 4H2O] 2 2CO2 + 2H+ +2e- ] 5 2Mn2+ + 10CO2 + 8H2O

2 moles of KMnO4 5 moles of (COOH)2 No external indicator is used as the colour of KMnO4 acts as the indicator.

PROCEDURE: 1. Praparation of around 0.02 M potassium permanganate solution: Weigh out about 3.2- 3.5 g potassium permanganate, transfer it to a 1500 mL beaker. Add 1L water, cover the beaker with a watchglass, and heat the solution to boil, then boil gently for 1530 minutes and allow the solution to cool to laboratory temperature. Filter the solution through a sintered-glass crucible or funnel. Collect the filtrate in a clean glass vessel with stopper and keep in the dark except when in use. Alternatively, it may be kept in a dark brown glass bottle. 2. Preparation of standard oxalic acid (0.1M): Weigh out accurate 3.15 g of supplied dehydrate oxalic acid, (COOH)2.2H2O. (If the acid is anhydrous, i.e., containing no water molecule, take only 2.25 g of the acid.) Transfer the acid crystals into 250 cm3 volumetric flask and dissolve it in small amount (about 50 cm3) of water. Add more water (about 50 cm3), close the mouth properly with stopper (not with thumb!) Repeat the process of adding water and shaking the solution until the level of solution touches the neck of the flask. Now add water carefully (for this you can use clean pipette) to make up the index mark (lower meniscus of the solution should touch the index mark).Be careful not to cross the index mark. Shake the flask well to make the solution homogeneous. 3. Preparation of 1M sulphuric acid: Prepare by dilution method, an aqueous solution of H2SO4 around 1M in desired volume by the knowledge of sp.gr., % purity and formula weight of sulphuric acid. 4. Titration of KMnO4 solution with standard oxalic solution in acidic medium: First of all, wash the burette with distilled water then rinse it with KMnO4 solution and finally fill it with KMnO4 solution and note down the initial reading of burette looking at the upper meniscus of the solution since the solution is coloured and difficult to see its lower meniscus. Pipette out 10 mL of the standard oxalic acid and transfer it to a conical flask .Mix this solution with 10 mL of dil H2SO4.Warm the solution (60 - 70 C) and this mixture is titrated with KMnO4 solution. Before end point pink colour of KMnO4 disappears but at the end point faint pink colour persists for 30 seconds. Repeat the process till you get at least two concurrent readings.By this method the concentration of potassium permanganate solution is determined. Now the standard solution of KMnO4 can be used to titrate other reducing agents like iron (II) ion, hydrogen peroxide.

OBSERVATION: Titration of standard oxalic acid solution Vs KMnO4 solution

Vol. of oxalic acid (ml) Using Pipette Concurrent reading, Vol. of KMnO4 solution consumed (ml)

No. of obs.

Initial burette reading (ml)

Final burette reading (ml)

Difference of burette reading (ml)

SUMMARY: 10 cm3 of 0.1M Oxalic acid solution required _________ cm3 of KMnO4 solution. CALCULATIONS:

RESULT: The concentration of the given KMnO4 solution is ________ M, or, _______ g / dm3.

CONCLUSION:

PRECAUTIONS:

POSSIBLE SOURCES OF ERRORS :