A solid-phase extraction method using 4-(2-thiazolylazo) resorcinol (TAR) as chelating agent on Amberlite XAD-16 column has been used for separation/preconcentration of trace amounts of cobalt prior to its determination by atomic absorption spectrometry. Cobalt was retained on the Amberlite XAD-16 column at pH 6. Cobalt was desorbed from Amberlite XAD-16 by 1 M nitric acid in acetone. The effect of the various components of urine such as some anions and cations on the recovery of cobalt was also investigated. The method was applied to urine samples collected randomly selected six people living in Kayseri with satisfactory results (recovery > 95%; relative standard deviation 1 - 9%).