Zhang Nan, Suleiman Jibrin Sabo, He Man, Hu Bin
Department of Chemistry, Wuhan University, Wuhan, Hubei Province 430072, PR China.
Talanta. 2008 Apr 15;75(2):536-43. doi: 10.1016/j.talanta.2007.11.059. Epub 2007 Dec 4.
A new chromium(III)-imprinted 3-(2-aminoethylamino) propyltrimethoxysilane (AAPTS)-functionalized silica gel sorbent was synthesized by a surface imprinting technique and was employed as a selective solid-phase extraction material for speciation analysis of chromium in environmental water samples prior to its determination by inductively coupled plasma mass spectrometry (ICP-MS). The prepared Cr(III)-imprinted silica gel shows the selectivity coefficient of more than 700 for Cr(III) in the presence of Mn(II). The static adsorption capacity of the ion-imprinted and non-imprinted sorbent for Cr(III) were 30.5 mg g(-1) and 13.4 mg g(-1). It was also found that Cr(VI) could be adsorbed at low pH by the prepared imprinted silica gel, and this finding makes it feasible to enrich and determine Cr(VI) at low pH without adding reducing reagents. The imprinted silica gel sorbent offered a fast kinetics for the adsorption and desorption of both chromium species. Under the optimized conditions, the detection limits of 4.43 pg mL(-1) and 8.30 pg mL(-1) with the relative standard deviations (R.S.D.s) of 4.44% and 4.41% (C=0.5 ng mL(-1), n=7) for Cr(III) and Cr(VI) were obtained, respectively. The proposed method was successfully applied to the speciation of trace chromium in environmental water samples. To validate the proposed method, two certified reference materials were analyzed and the determined values were in a good agreement with the certified values. The developed method is rapid, selective, sensitive and applicable for the speciation of trace chromium in environmental water samples.
通过表面印迹技术合成了一种新型的铬(III)印迹3-(2-氨乙基氨基)丙基三甲氧基硅烷(AAPTS)功能化硅胶吸附剂,并将其用作环境水样中铬形态分析的选择性固相萃取材料,用于电感耦合等离子体质谱(ICP-MS)测定之前的样品处理。制备的铬(III)印迹硅胶在锰(II)存在下对铬(III)的选择性系数超过700。离子印迹和非印迹吸附剂对铬(III)的静态吸附容量分别为30.5 mg g⁻¹和13.4 mg g⁻¹。还发现制备的印迹硅胶在低pH值下可以吸附铬(VI),这一发现使得在不添加还原剂的情况下在低pH值下富集和测定铬(VI)成为可能。印迹硅胶吸附剂对两种铬形态的吸附和解吸都具有快速动力学。在优化条件下,铬(III)和铬(VI)的检测限分别为4.43 pg mL⁻¹和8.30 pg mL⁻¹,相对标准偏差(R.S.D.s)分别为4.44%和4.41%(C = 0.5 ng mL⁻¹,n = 7)。所提出的方法成功应用于环境水样中痕量铬的形态分析。为了验证所提出的方法,分析了两种有证标准物质,测定值与认证值吻合良好。所建立的方法快速、选择性好、灵敏,适用于环境水样中痕量铬的形态分析。