The present work focuses on the preconcentration of molybdenum and its determination in aqueous solutions by means of diffuse reflection spectroscopy. The preconcentration of Mo(VI) was carried out using the macroporous strong basic anion exchanger AV-17-10P synthesized on the basis of styrene and divinylbenzene. The method for Mo determination with this collector in industrial solutions and natural water was developed using solid-phase spectroscopy. The colored surface compound to be determined was obtained by a preceding Mo(VI) sorption on the resin and by subsequent treatment of the concentrate obtained with definite amounts of pyrocatechol violet. The calibration curve is linear at the Mo (VI) concentration range 0.05-2.5 mg(.)dm(-3) with a sample volume of 50.0 cm(3). The detection limit is 0.002 mg.dm(-3).