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Explain Kjeldahl’s method.

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Principle:

This method is based on the fact that an organic compound containing nitrogen is heated with cone. H2SO4 . the nitrogen is converted to ammonium sulphate. The resultant liquid is heated with excess of alkali and then liberated ammonia gas is absorbed in excess of standard acid. The amount of ammonia (nitrogen) is determined by finding the amount of acid neutralised by back titration with same standard alkali.

Procedure:

A weighed quantity of the substance 0.3 to 0.5 g is placed in a special long necked Kjeldahl flask made of pyrex glass. About 25 ml of cone. H2SO4 together with a little K2SO4 and CuSO4 [catalyst] are added to it. the flask is loosely stoppered by a glass bulb and heated gently in an inclined position.

The heating is continued till the brown colour of the liquid disappears leaving the content clear as before. At this point all the nitrogen is converted to ammonium sulphate. The kjeldahl flask is cooled and its contents are diluted with distilled water and carefully transferred into a I litre round bottom flask. An excess NaOH is poured down the side of the flask and it is filled with a kjeldhals trap and a water condenser.

The lower end of the condenser dips in a measured volume of excess of \(\frac{N}{20}\) H2SO4 solution. The liquid in the round bottom flask is heated and liberated ammonia is distilled to sulphuric acid. When no more ammonia passes over (test the distillate with red litmus) the receiver is removed. The excess of acid is then determined by titration with alkali, using phenolphthalein as the indicator.

Calculation:

Weight of the substance = Wg

Volume of H2SO4 required for the complete neutralisation of evolved NH3 = V ml

Strength H2SO4 used to neutralise NH3 = N.

Let the volume and strength of NH3 formed are V1 and N1 respectively.

V1N1 = VN

The amount of nitrogen present in W g of organic compound = Extra close brace or missing open brace

Percentage of nitrogen = \(\frac{14\times NV}{1000\times w}\times100\) = \(\frac{1.4NV}{w}\%\)

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