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合成了新试剂 5 ,7-二溴〔杯 ( 4 )芳烃偶氮〕氨基喹啉 (DBCAQ) ,经红外光谱、元素分析和薄板层析检验其结构。研究了该试剂与Pd(Ⅱ )的显色反应的适宜条件。在pH =5 0的HAc -NaAc缓冲溶液中及非离子表面活性剂吐温 - 80存在下 ,试剂与Pd(Ⅱ )生成 1∶1的稳定配合物 ,建立了测定Pd(Ⅱ )的光度法新体系 ,该体系至少可稳定 1 0h ,λmax=680nm ,ε =8 2 6× 1 0 4 L/mol·cm ,Pd(Ⅱ )浓度在 0～ 35 μm/2 5ml内服从比耳定律。方法已用于钯催化剂中Pd(Ⅱ )的测定 ,结果与原子吸收法 (AAS)结果相符。
A new reagent, 5, 7 - dibromo [calix [4] arene] aminoquinoline (DBCAQ) was synthesized and its structure was confirmed by IR, elemental analysis and thin layer chromatography. The suitable conditions for the color reaction of this reagent with Pd (Ⅱ) were studied. A stable 1: 1 complex was prepared with Pd (Ⅱ) in the presence of non-ionic surfactant Tween-80 at pH = 50 in HAc-NaAc buffer solution. A spectrophotometric method for the determination of Pd The new system can stabilize at least 10h, λmax = 680nm, ε = 8 2 6 × 10 4 L / mol · cm and Beer’s Law obey Beer’s Law within the range of 0 ~ 35 μm / The method has been applied to the determination of Pd (Ⅱ) in palladium catalysts. The results are consistent with the results of atomic absorption spectrometry (AAS).