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本文提出一种新的测定铑的催化氢波体系.先使Rh(Ⅲ)与3,5-diCl-PADMA在HAc-NaAc缓冲溶液中生成稳定的络合物,再以适量HclO_4将溶液酸化后进行极谱测定。利用正交试验法确定体系的最佳分析条件为:0.05 mol/L pH5.0的HAc-NaAc,1.6×10~(-5)mol/L3,5-diCl-PADMA,沸水浴加热15min.,4.4 mol/L HCIO4酸化。在此条件下的线性范围为1.9×10~(-11)～3.9×10~(-9)mol/L,检出限达5.8×10~(-12)mol/L。大量Cu(Ⅱ)、Ni(Ⅱ)、Fe(Ⅲ)及Co(Ⅱ)对体系的干扰可用EDTA消除。研究了催化波的性质,表明该波为Rh(Ⅲ)与3,5-diClPADMA络合物的催化氢波。
In this paper, a new catalytic hydrogen wave system for the determination of rhodium is proposed. After Rh (Ⅲ) and 3,5-diCl-PADMA form a stable complex in HAc-NaAc buffer solution, the solution is acidified with appropriate amount of HclO 4 Polarographic determination. The optimum conditions for the determination of the system by orthogonal test were as follows: 0.05 mol / L HAc-NaAc at pH 5.0, 1.6 × 10 -5 mol / L 3,5-diCl-PADMA, 4.4 mol / L HCIO4 acidified. Under these conditions, the linear range was 1.9 × 10 ~ (-11) ~ 3.9 × 10 ~ (-9) mol / L with a detection limit of 5.8 × 10 ~ (-12) mol / L. A large number of Cu (Ⅱ), Ni (Ⅱ), Fe (Ⅲ) and Co (Ⅱ) interference of the system can be eliminated with EDTA. The nature of the catalytic wave was investigated, indicating that this wave is a catalytic hydrogen wave of Rh (Ⅲ) complex with 3,5-diClPADMA complex.