异戊基亚砜树脂固相萃取原子吸收光谱法测定催化剂中钯  

Determination of palladium in catalysts by atomic absorption spectrometry after solid phase extraction with isopentyl sulfoxide resin

作　　者：黄章杰[1,2] 王世雄[1] 谢琦莹[1] 

机构地区：[1]云南大学化学系,云南昆明650091 [2]昆明理工大学材料与冶金工程学院,云南昆明650093

出　　处：《冶金分析》2009年第1期17-20,共4页Metallurgical Analysis

基　　金：国家自然科学基金(50764008);云南省自然科学基金重点项目(2005E0003Z);国家863项目(2006AA06Z127)

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0．1～2．0mol／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20g／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。培养出异戊基亚砜一钯络合物单晶，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％。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 HC1 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.

关 键 词：固相萃取 异戊基亚砜树脂 钯 原子吸收光谱法 

分 类 号：O657.31[理学—分析化学]