Discuss the principle of estimation of halogens, sulphur and phosphorus present in an organic compound.
Estimation of phosphorus:
A known mass of an organic compound is heated with fuming nitric acid whereupon phosphorus present in the compound is oxidised to phosphoric acid. It is precipitated as ammonium phosphomolybdate, (NH4)3 PO4.12MoO3, by adding ammonia and ammonium molybdate. Alternatively, phosphoric acid may be precipitated as MgNH4PO4 by adding magnesia mixture which on ignition yields Mg2P2O7.
Estimation of halogens:
Carius method: A known mass of an organic compound is heated with fuming nitric acid in the presence of silver nitrate contained in a hard glass tube known as Carius tube, in a furnace. Carbon and hydrogen present in the compound are oxidised to carbon dioxide and water. The halogen present forms the corresponding silver halide (AgX). It is filtered, washed, dried and weighed.
Estimation of sulphur:
A known mass of an organic compound is heated in a Carius tube with sodium peroxide or fuming nitric acid. Sulphur present in the compound is oxidised to sulphuric acid. It is precipitated as barium sulphate by adding an excess of barium chloride solution in water. The precipitate is filtered, washed, dried and weighed.