【摘要】 基于异戊基亚砜树脂与钯的络合反应,建立了一种高选择性固相萃取测定痕量钯的方法。在0.1~2.0 mol/L的盐酸介质中,钯可以被异戊基亚砜树脂吸附富集并形成1∶2稳定络合物,该络合物可用20 g/L酸性硫脲洗脱,洗脱液用火焰原子吸收光谱法直接测定,树脂结构不被破坏且可重新处理使用。培养出异戊基亚砜-钯络合物单晶,实现了从分子结构水平上解释异戊基亚砜树脂萃取钯的机理。方法用于测定催化剂中痕量钯,结果与ICP-AES法一致,相对标准偏差(RSD)为2.4%~3.2%(n=7),标准加入回收率为98%~101%。更多还原

【Abstract】 On the basis of the complex reaction of isopentyl sulfoxide resin with palladium,a high-selective method of solid phase extraction for the determination of trace palladium was developed.In 0.1-2.0 mol/L HCl medium,palladium could be adsorbed and enriched by isopentyl sulfoxide resin and a stable complex with ratio of 1∶2 was formed.The complex could be eluted by 20 g/L of acidic thiourea.The eluent was determined directly by flame atomic absorption spectrometry,and the structure of resin was kept well,which could be retreated and reused readily.The single crystal of isopentyl sulfoxide-palladium complex was obtained,explaining the mechanism of extracting palladium from molecule structure level.The method has been applied to the determination of trace palladium in catalysts with RSD of 2.4%-3.2%(n=7) and recovery of 98%-101%.The results were consistent with those obtained by ICP-AES method.更多还原