基于以柠檬酸为活化剂,在硫酸介质中钒(Ⅴ)能灵敏地催化高碘酸钾氧化结晶紫的褪色反应,建立了一种测定痕量钒(Ⅴ)新催化光度分析方法.在最佳实验条件下,催化反应吸光度与非催化反应吸光度的差值△A与V(Ⅴ)的质量浓度(ρ)在0～0.06 μg/mL范围内呈良好的线性关系,方法的检出限为5.421×10~(-10)g/mL.对0.04μg/mL V(Ⅴ)测定的相对标准偏差为1.2%(n=11).该催化反应对钒(Ⅴ)为一级反应,总反应为准一级反应,表观速率常数为2.055×10~(-4)/s,表观活化能为50.05 kJ/mol.方法用于炼钢烧结矿样品中痕量钒(Ⅴ)的测定,回收率在100%～101%之间.
This paper focused on the determination of trace vanadium(Ⅴ) by catalytic kinetic spectropho-tometric method. Based on its oxidative fading reaction of crystal violet and potassium periodate in sulfuric acid medium, a new method for the determination of trace vanadium was established in the presence of citric acid as activator. The mass concentration of vanadium(Ⅴ) p remained good linear rela-tionship with △A in the range of 0-0.06 μg/mL. The detection limit was 5.421 ×10~(-4) μg/mL. Rela-tive standard deviation of the determination of 0. 04 μg/mL V(V) RSD was 1.24 % (n=11). The cat-alytic reaction was first-order reaction. The whole reaction was pseudo first order reaction. The appar-ent ratio constant was 2. 055×10~(-4)/s and the apparent active energy was 50.05 kJ/mol. The method is of good selectivity and high sensitivity. The recovery ratio was between 100%-101% in the determi-nation of trace vanadium(Ⅴ) in sample sinter steel.
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