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本文建立了一种催化极谱法测定痕量铑的新方法.先使铑(Ⅲ)与5-Cl-PADAT在pH5的HOAc-NaOAc缓冲溶液中生成稳定的配合物,再于适量HClO_4底液中进行极谱测定.并研究了影响极谱催化波的各种因素及波的性质,确定该波为铑(Ⅲ)与5-Cl-PADAT配合物的催化氢波,提出了可能的电极过程,并进行了实验验证.该法测定铑的线性范围为3.9×10~(12)—3.9×10~(-9)mol·dm~(-3),检出限为1.9×10~(-12)mol·dm~(-3).已应用于镍基合金及催化剂中铑的测定.
In this paper, a new method for the determination of trace rhodium by catalytic polarography was established. First, rhodium (Ⅲ) was reacted with 5-Cl-PADAT in HOAc-NaOAc buffer at pH5 to form a stable complex. , And studied the various factors affecting the polarographic catalytic wave and the nature of the wave, and determined the catalytic hydrogen wave of the rhodium (III) complex with 5-Cl-PADAT, and proposed a possible electrode process The experimental results show that the linear range of rhodium is 3.9 × 10 ~ (12) -3.9 × 10 ~ (-9) mol · dm -3 and the detection limit is 1.9 × 10 ~ (- 12) mol · dm ~ (-3). It has been applied to the determination of rhodium in nickel base alloys and catalysts.