Determination of persulphates

Discussion. Alkali persulphates (peroxydisulphates) can readily be evaluated by adding to their solutions a known excess of an acidified iron(II) salt solution, and determining the excess of iron(II) by titration with standard potassium permanganate solution. 

By adding phosphoric acid or hydrofluoric acid, the reduction is complete in a few minutes at room temperature. Many organic compounds interfere. 

Another procedure utilises standard oxalic acid solution. When a sulphuric acid solution of a persulphate is treated with excess of standard oxalic acid solution in the presence of a little silver sulphate as catalyst, the following reaction occurs  

The excess of oxalic acid is titrated with standard potassium permanganate solution. 

Procedure A. Prepare an approximately 0.1 JVf solution of ammonium iron(II) sulphate by dissolving about 9.8 g of the solid in 200 mL of sulphuric acid (0.5M) in a 250 mL graduated flask, and then making up to the mark with freshly boiled and cooled distilled water. Standardise the solution by titrating 25 mL portions with standard potassium permanganate solution (0.02M) after the addition of 25 mL sulphuric acid (0.5JVf). 

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