A method is proposed for the simultaneous determination of iron(III) and molybdenum(VI) by first-derivative spectrophotometry based on the absorption spectra of their complexes with morin in the presence of a cationic surfactant. The zero-crossing measurement technique is found sutiable for the direct measurement of the first-derivative value at the specified wavelengths. Iron(III) (0.9-1.5 mu g ml(-1)) and molybdenum(VI) (0.3-4.2 mu g ml(-1)) in different ratios have been determined simultaneously. A critical evaluation of the proposed method is performed by statistical analysis of the experimental data. The method was applied to determine iron and molybdenum in different alloys.