The formation of [FeSCN](2+)complex in hydrochloric and sulfuric acid medium was studied by spectrophotometry using iron(III) sulfate and ammonium iron(III) sulfate solutions as reactants. A method for the determination of 10-200 mu g SCN-in 25 mL water solutions containing ammonium iron(III) sulfate in sulfuric acid medium was developed; its determination limit is 2.6 mu g (P = 0.99, n = 9). The method was applied for the analysis of model water samples with macro-and micro-component compositions similar to that of water from the Arigol licensed area. Operational control of the accuracy rate was performed by the standard addition method. The developed method can be applied to analyze water samples containing 1-90 mg/L thiocyanate ions.