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A simple and reliable method for the selective extraction and determination of bismuth in water as well as alloy samples using octadecyl bonded silica cartridge modified with cyanex 301 and graphite furnace atomic absorption spectrometry is described. Extraction efficiency and influence of sample matrix, optimum amount of extraction ligand, type and least amount of proper eluent and flow rates were evaluated. The limit of detection of the proposed method is 0.01 ng ml⁻¹. The influence of potential interfering cations in water samples on the recovery of bismuth was investigated. The method was successfully applied to the extraction and determination of bismuth in natural water and alloy samples.