On-line spectrophotometric determination of scandium after preconcentration on XAD-4 resin impregnated with nalidixic acid

Abstract

An on-line scandium preconcentration and determination method was developed with spectrophotometer associated with flow injection. Scandium from aqueous sample solution of pH 4.5 was selectively retained in the minicolumn containing XAD-4 resin impregnated with nalidixic acid at a flow rate of 11.8 mL min−1 as scandium–nalidixic acid complex. The scandium complex was desorbed from the resin by 0.1 mol L−1 HCl at a flow rate of 3.2 mL min−1 and mixed with arsenazo-III solution (0.05 % solution in 0.1 mol L−1 HCl, 3.2 mL min−1) and taken to the flow through cell of spectrophotometer where its absorbance was measured at 640 nm. The preconcentration factors obtained were 35 and 155; detection limits of 1.4 and 0.32 μg L−1 and sample throughputs of 40 and 11 were obtained for preconcentration time of 60 and 300 s, respectively. The tolerance limits of many interfering cations like Th(IV), U (VI), rare-earths and anions like tartrate, citrate, oxalate and fluoride were improved. The method was successfully applied to the determination of scandium from mock seawater samples and good recovery was obtained. The method was also validated on certified reference material IAEA-SL-1 (lake sediment) and the result was in good agreement with the reported value.