The concentration of lead, nickel, copper and cadmium in the water samples collected from Tabakhane River and Akkaya Dam (Nigde City-Turkey) have been determined by graphite furnace atomic absorption spectrometry after preconcentration and separation by sorbing the metal/4-(2-Thiazolylazo) resorcinol complexes on an activated carbon column. The concentration ranges of lead, copper and cadmium were 1.1-4.9 mu g/l, 0.7-2.5 mu g/l and 0.3-1.3 mu g/l respectively. The nickel content of the samples was below 1 mu g/l. The metal contents of the water samples were below the values given in the Water Pollution Control Regulation of Turkish Authorities. The metal contents of the sediment samples have been also determined by flame atomic absorption spectrometry after digestion procedure with aqua regia.