A simple adsorptive cathodic stripping voltammetry method has been developed for antimony (III and V) speciation using 4-(2-thiazolylazo) -resorcinol (TAR). The methodology involves controlled preconcentration at pH 5, during which antimony(III) -TAR complex is adsorbed onto a hanging mercury drop electrode followed by measuring the cathodic peak current (I p,c ) at À0.39 V versus Ag/AgCl electrode. The plot of I p,c versus antimony(III) concentration was linear in the range 1.35 10 À9 -9.53 10 À8 mol L
À1.The LOD and LOQ for Sb(III) were found 4.06 10 À10 and 1.35 10 À9 mol L
À1, respectively. Antimony(V) species after reduction to antimony(III) with Na 2 SO 3 were also determined. Analysis of antimony in environment water samples was applied satisfactorily.