Determination of semicarbazide using photochemical exchange reaction of sodium nitroprusside has been investigated. It is an inexpensive, faster and convenient quantitative method. Sodium nitroprusside is a photolabile complex, which undergoes photochemical ligand exchange reactions rapidly. Some recent efforts have been made to utilise such reactions for the estimation of some nitrogen containing anions and electron rich organic molecules. The progress of the reaction is observed spectrophotometrically. The effects of different parameters like pH, change of concentration of sodium nitroprusside, concentration of ligands, light intensity etc. on percentage error was investigated. The efforts were made to minimise the percentage error and optimum conditions were obtained. Such reaction can be used for the determination of semicarbazide in the range of millimoles to micromoles; and that too with the desired accuracy.