Catalytic Determination of Vanadium Based on the Bromate Oxidative-C oupling Reaction of Metol with Phloroglucinol

 A selective, sensitive and simple catalytic method is developed for the determination of vanadium in natural and highly polluted waste waters. The method is based on the catalytic effect of VV and/or VIV on the bromate oxidative-coupling reaction of metol with phloroglucinol (PG). The reaction is followed spectrophotometrically by tracing the oxidation product at 464 nm after 10 minutes of mixing the reagents. The optimum reaction conditions are metol (8.0×10−3 M), PG (4.0×10−3 M) and bromate (2×10−2 M) at 35°C and in presence of an activator-b uffer mixture of 5×10−2 M of each of citric and monochloroacetic acids (pH 2.40). Following the recommended procedure, vanadium can be determined with a linear calibration graph up to 8.0 ng mL−1 and a detection limit, based on the 3sb criterion, of 0.1 ng mL−1. Spectrophotometric determination of as little as 1.0 ng mL−1 of VV or VIV in aqueous solutions gave an average recovery of 98% with relative standard deviations of ?1.8% (n = 5). The proposed method was directly applied to the determination of vanadium in Nile river water and highly polluted industrial wastes. Statistical treatments of analytical results could not detect any systematic error and showed the high accuracy and precision of the developed method.