He Qun, Chang Xijun, Wu Qiong, Huang Xinping, Hu Zheng, Zhai Yunhui
Department of Chemistry, Lanzhou University, Lanzhou 730000, PR China.
Anal Chim Acta. 2007 Dec 19;605(2):192-7. doi: 10.1016/j.aca.2007.10.026. Epub 2007 Oct 24.
A new functional monomer N-(o-carboxyphenyl)maleamic acid (CPMA) was synthesized and chosen for the preparation of surface-grafted ion-imprinted polymers (IIPs) specific for thorium(IV). Polymerizable double bond was introduced to silica gel surface by amidation reaction between -NH2 and maleic anhydride. In the ion-imprinting process, thorium(IV) was complexed with the carboxyl groups, then was imprinted in the polymers grafted to the silica gel surface. The imprinted Th(IV) was removed with 3 mol L(-1) HCl. The obtained imprinted particles exhibited excellent selectivity and rapid kinetics process for Th(IV). The relatively selective factor (alpha(r)) values of Th(IV)/La(III), Th(IV)/Ce(III), Th(IV)/Nd(III), Th(IV)/U(VI), and Th(IV)/Zr(IV) were 85.7, 88.9, 26.6, 64.4, and 433.8, respectively, which were greater than 1. The precision (R.S.D.), the detection limit (3sigma), and the quantification limit (10sigma) of the method were 1.9%, 0.51 ng mL(-1) and 1.19 ng mL(-1), respectively. The prepared IIPs as solid-phase extractants were successfully applied for the preconcentration of trace thorium in natural and certified samples prior to its determination by inductively coupled plasma atomic emission spectrometry (ICP-AES) with satisfactory results.
合成了一种新型功能单体N-(邻羧基苯基)马来酰胺酸(CPMA),并将其用于制备对钍(IV)具有特异性的表面接枝离子印迹聚合物(IIPs)。通过-NH2与马来酸酐之间的酰胺化反应将可聚合双键引入硅胶表面。在离子印迹过程中,钍(IV)与羧基络合,然后被印迹在接枝到硅胶表面的聚合物中。用3 mol L(-1) HCl去除印迹的Th(IV)。所得印迹颗粒对Th(IV)表现出优异的选择性和快速动力学过程。Th(IV)/La(III)、Th(IV)/Ce(III)、Th(IV)/Nd(III)、Th(IV)/U(VI)和Th(IV)/Zr(IV)的相对选择性因子(α(r))值分别为85.7、88.9、26.6、64.4和433.8,均大于1。该方法的精密度(R.S.D.)、检测限(3σ)和定量限(10σ)分别为1.9%、0.51 ng mL(-1)和1.19 ng mL(-1)。所制备的IIPs作为固相萃取剂成功应用于天然样品和标准样品中痕量钍的预富集,然后通过电感耦合等离子体原子发射光谱法(ICP-AES)进行测定,结果令人满意。