借4-(2-噻唑偶氮)间苯二酚螯合物和反相高压液相色谱法以分离和测定钒、钴和铬

On Separation and Deteimination of Vanadium, Cobalt and Chromium as Chelates with 4-(2-Thiazolylazo) resorcinol by Reversed-phase HPLC

研究了V(Ⅴ)、Co(Ⅱ)和Cr(Ⅲ)的TAR螯合物的柱前衍生条件和反相高压液相色谱分离条件,并提出了同时测定ppb级的此三元素的新方法.于Zorbax ODS柱上,用含0.05mol·dm^(-3)Li_2SO_4和0.01mol·dm^(-3)HOAc-NaOAc(pH 6.0)的46∶54甲醇-水(v/v)溶液作流动相(0.7mL/min),可于15min内将此三螯合物分离并检测(525nm)完毕.此方法快速、经济、灵敏选择性好.

The cited chelates were separated on a column (250×4.6mm) of Zorbax ODS (6μm) with a mobile phase (0.7mL/min) of 46:54 methanol-water (v/v) containing 0.05mol·dm^(-3) lithium sulphate and 0.01 mol·dm^(-3) acetio acid-sodium acetate buffer (pH6.0). Detection was made at 525nm. The calibration graphs were rectilinear from 0.025 to 4.0 ppm for both V and Cr, and 0.025 to 2.0 ppm for Co. Detection lim(?)ts were 0.62ng for V, 0.35ng for Cr and 0.23ng for Co. Tolerable amounts (in μg) of foreign ions were: Al(Ⅲ) 20, Ca(Ⅱ) 100, Cd(Ⅱ) 40, Cu(Ⅱ) 10, Fe(Ⅱ) 10, Hg (Ⅱ) 30, Mg(Ⅱ) 100, Mn(Ⅱ) 50, Mo(Ⅳ) 5, Ni(Ⅱ) 10, Pb(Ⅱ) 40, W(Ⅵ) 40, and Zn(Ⅱ) 20.