Automated in-chip kinetic-catalytic method for molybdenum determination

Abstract

In this work, the automation of a catalytic spectrophotometric method for the determination of molybdenum is presented. For this purpose, a multisyringe flow injection system was coupled to an integrated microconduit that we have called "chip". Reagents and sample were simultaneously dispensed to the chip where complete mixing, heating, and measurement were carried out. The spectrophotometric method is based on the oxidation of 4-amino-3-hydroxy- naphthalenesulphonic acid (AHNA) by hydrogen peroxide catalyzed by Mo (VI). Absorbance of the reaction product was measured at 465 nm. Two optical fibers were used to conduct the light, one from the source to the chip, and the other from the output of the cell to the spectrophotometer. The detection cell was incorporated in the thermostated zone of the chip. The initial rate method, at controlled temperature, was employed to determine the Mo (VI) concentration. The estimated precision was 3.7%, with the working range of 4.0-40 μg L-1of Mo (VI), and the limit of detection of 1.2 μg L-1of Mo (VI). The system was successfully applied to water samples and pharmaceutical products with a sampling throughput of 20 injections h-1. © 2013 Elsevier B.V.