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本文报道一种测定钒试剂的单扫描示波极谱法,它是基于在较浓的乙酸介质中钒试剂与亚硝酸盐作用迅速亚硝化,然后用极谱法对其亚硝化产物进行定量测定。本文研究了钒试剂亚硝化和测定的条件。实验表明,在4%乙酸-0.12mol/1.H_2SO_4 4×10~(-5)(4.8×10~(-4)、1.2×10~(-3))mol/L NaNO_2底液中,钒试剂亚硝化产物的极谱还原波波高与钒试剂浓度在4.0×10~(-7)mol/L~1.2×10~(-4)mol/L范围内有良好的线性关系,检测下限为1×10~(-7)mol/L。合成钒试剂的原料杂质如邻氯苯甲酸、苯胺和Cu~(2-)、Ni~(2+)、Zn~(2+)等不干扰测定。
In this paper, we report a single-scan oscillopolarographic method for the determination of vanadium reagents based on the rapid nitrosation of vanadium reagents with nitrite in a more concentrated acetic acid medium followed by the polarographic determination of their nitrosated products . In this paper, the conditions of nitrosation and determination of vanadium reagent were studied. The experimental results showed that in the 4% acetic acid -0.12mol / 1.H 2 SO 4 4 × 10 -5 (4.8 × 10 -4) and 1.2 × 10 -3 mol / L NaNO 2 solution, vanadium The polarographic reduction wave height of the reagent nitrosation products has a good linear relationship with the vanadium reagent concentration in the range of 4.0 × 10 -7 mol / L to 1.2 × 10 -4 mol / L with the detection limit of 1 × 10 ~ (-7) mol / L. Raw materials such as o-chlorobenzoic acid, aniline and Cu2 +, Ni2 +, Zn2 + and so on did not interfere with the determination of vanadium reagent.