DETERMINATION OF ZIRCONIUM AND MOLYBDENUM WITH 4,5-DIHYDROXYBENZENE-1,3-DISULFONIC ACID DISODIUM SALT BY ION-PAIR REVERSED-PHASE HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY
Sjj. Tsai et Ht. Yan, DETERMINATION OF ZIRCONIUM AND MOLYBDENUM WITH 4,5-DIHYDROXYBENZENE-1,3-DISULFONIC ACID DISODIUM SALT BY ION-PAIR REVERSED-PHASE HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY, Analyst, 118(5), 1993, pp. 521-527
An analytical process based on reversed-phase high-performance liquid
chromatography, with ultraviolet/visible detection at 315 nm, was stud
ied. 4,5-Dihydroxybenzene-1,3-disulfonic acid disodium salt (Tiron) wa
s used as chelating agent. Optimum conditions for the determination of
zirconium and molybdenum ions, including the concentration of the buf
fer, the pH of the chelating medium and the mobile phase, the concentr
ation of Tiron, the time of colour development and the composition of
the mobile phase, were investigated. Tiron chelates were eluted within
15 min, with methanol-water (63 + 37) as the mobile phase, which cont
ained acetate buffer (1.5 x 10(-3) mol l-1, pH 4.0), Tiron (1.5 x 10(-
3) mol l-1) and tetrabutylammonium bromide (3 X 10(-2) mol l-1). The s
eparation was performed with a C18 reversed-phase column. The proposed
method was applied to the determination of Zr(IV) and Mo(VI) in a rel
atively complex substance, nickel-base alloy. The precision and accura
cy of the method were evaluated. The experimental values obtained from
the calibration graphs and by the standard additions method were comp
ared with the certified values. There was good agreement between these
values. With five consecutive injections of 100 mul of sample solutio
n, containing 200 ng each of Zr(IV) and Mo(VI), the recoveries obtaine
d for Zr and Mo were 97 and 106%, respectively. The detection limits (
signal-to-noise ratio = 3) were 9.0 and 3.6 ppb for Zr(IV)-Tiron and M
o(VI)-Tiron, respectively.