A kinetic method for the determination of micro quantities of diclofenac sodium (DS) is described in this paper. The method is based on a ligand-exchange reaction. The reaction was followed spectrophotometrically by monitoring the rate of appearance of the cobalt diclofenac complex at 376 nm. The optimum operating conditions regarding reagent concentrations and temperature were established. The optimized conditions yielded a theoretical detection limit of 1.29 μg ml⁻¹ based on the 3S_b criterion. The interference effects of certain drugs, foreign ions and amino acids upon the reaction rate were studied in order to assess the selectivity of the method. The developed procedure was successfully applied to the rapid determination of diclofenac sodium in commercial pharmaceutical preparations and human control serum. The unique features of this procedure are that determination can be carried out at room temperature and the analysis time is short. The newly developed method is simple, inexpensive, and efficient for use in the analysis of a large number of samples.