SPECIATION OF VANADIUM(V) AND VANADIUM(IV) WITH 4-(2-PYRIDYLAZO)RESORCINOL BY USING HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY WITH SPECTROPHOTOMETRIC DETECTION

By using 4-(2-pyridylazo)resorcinol (PAR) as the chelating reagent, va nadate and vanadyl ions were effectively separated by reversed-phase h igh-performance liquid chromatography with ultraviolet-visible detecti on at 540 nm. The optimum conditions for the determination of these me tal ions were established. PAR chelates were eluted within 10 min with methanol-water (30 + 70 v/v) as the mobile phase containing acetate b uffer (8.0 x 10(-3) mol l-1, pH 6.0) and PAR (3.0 x 10(-4) mol l-1). T he retention times for V(V) and V(IV) were 4.91 and 9.01 min, respecti vely. The calibration graphs obtained for 100 mul samples were linear for 0.02-2.00 mug ml-1 vanadium. The detection limits were 0.2 and 0.1 ng per 100 mul sample volume for V(V) and V(IV), respectively. The pr oposed method for the simultaneous speciation of vanadate and vanadyl ions was used to analyse a used vanadium-containing catalyst and good results were obtained in terms of precision and accuracy.