Abstract Trace amounts of molybdenum(VI) can be determined by the use of their catalytic effects on the peroxoborate–iodide redox reaction in acidic medium. The indicator reaction is transformed to a Landolt reaction by the addition of ascorbic acid into the reaction mixture, i.e., the iodine produced by the reaction is immediately reduced by ascorbic acid. The end of the induction period of the Landolt process was fluorometrically detected by the aid of disappearence of fluorescence of Rhodamine B. Trace determination of molybdenum(VI) was carried out by employing the linear relationship between the reciprocal of induction period and catalyst concentration. The most suitable concentrations of sodium peroxoborate, potassium iodide, and hydrochloric acid in the reaction mixture were found to be 9 mM, 0.1 M, and 0.1 M, respectively. By this method, molybdenum(VI) can be determined from 80 nM to 10 mM (7.675 ng ml−1 to 95.95 mg ml−1). The effect of foreign ions were studied and an equal amount of tungsten(VI), and 10-fold amounts of zirconium(IV), iron(II), iron(III), vanadium(IV), and copper(II) were found to show interference. Ascorbic acid and thiosulfate in micro mol l−1 levels were also determined by the present method employing the linear relationship between the induction period and the reductant concentration.
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