Abstract
A selective method for the spectrophotometric determination of V in the presence of other refractory elements is proposed. It is based on the re-examination of its redox reaction with 2,2′-iminodibenzoic acid in H2SO4 medium (11.1–11.4 mol l–1) in the presence of H3PO4. Up to 1 mg of TiIV, ZrIV, NbV, MoVI and WVI do not interfere. V should be pre-oxidized in H2SO4 medium (⩽6.5 mol l–1) at room temperature with a 0.1% m/v solution of potassium permanganate, the excess of which is removed by adding successively 1 ml of a 10% m/v solution of urea and a few drops of a 0.1% solution of sodium nitrite. The molar absorptivity of this system was found to be 1.2 × 104 l mol–1 cm–1 at 610 nm. The Lambert–Beer law is obeyed over the concentration range 0.4–2.0 µg ml–1 of V with the linear regression equation A= 0.0188C–0.0229 (C=µg of V per 25 ml) and correlation coefficient r= 0.9990. The standard deviation (n= 10) and relative standard deviation at the level of 20 µg of V were found to be 0.88 µg and 4.4%, respectively. The versatility of the proposed method was demonstrated by incorporation of the preconcentration of V with N-benzoyl-N-phenylhydroxylamine as precipitant and MoVI as carrier.
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