Zhang Lijun, Chang Xijun, Zhai Yunhui, He Qun, Huang Xinping, Hu Zheng, Jiang Na
Department of Chemistry, Lanzhou University, Tianshui Road 222, Lanzhou 730000, PR China.
Anal Chim Acta. 2008 Nov 23;629(1-2):84-91. doi: 10.1016/j.aca.2008.09.039. Epub 2008 Sep 21.
In this study, a new 4-(2-morinyldiazenyl)-N-(3-(trimethylsilyl)propyl)benzamide modified silica gel (SG-MTPB) sorbent was prepared and characterized by FT-IR spectroscopy and studied for separation and preconcentration of Sc(III) prior to its determination by inductively coupled plasma atomic emission spectrometry (ICP-AES). Experimental conditions for effective adsorption of trace Sc(III) were optimized using both batch and column procedures. At pH 3, Sc(III) could be quantitatively adsorbed on the new sorbent. And the adsorbed Sc(III) could be completely eluted by using 2 mL of 6 mol L(-1) of HCl+2% CS(NH(2))(2). Most common coexisting ions did not interfere with the separation and preconcentration of Sc(III) at optimal conditions. The maximum static adsorption capacity of the sorbent for Sc(III) was 600 micaromol g(-1) while the time of 95% adsorption was less than 2 min. The detection limit of present method was found to be 0.085 micarog g(-1), and the relative standard deviation (R.S.D.) was lower than 1.3%. The method was also successfully applied to the preconcentration of trace Sc(III) in the environmental samples with satisfactory results.
在本研究中，制备了一种新型的4-(2-吗啉基重氮基)-N-(3-(三甲基硅基)丙基)苯甲酰胺修饰硅胶（SG-MTPB）吸附剂，并用傅里叶变换红外光谱对其进行了表征。在通过电感耦合等离子体原子发射光谱法（ICP-AES）测定之前，研究了该吸附剂对Sc(III)的分离和预富集性能。采用分批和柱操作法优化了痕量Sc(III)有效吸附的实验条件。在pH 3时，Sc(III)可定量吸附在新型吸附剂上。吸附的Sc(III)可用2 mL 6 mol L(-1)的HCl + 2%硫脲完全洗脱。在最佳条件下，大多数常见共存离子不干扰Sc(III)的分离和预富集。该吸附剂对Sc(III)的最大静态吸附容量为600 μmol g(-1)，而95%吸附所需时间小于2 min。本方法的检出限为0.085 μg g(-1)，相对标准偏差（R.S.D.）低于1.3%。该方法也成功应用于环境样品中痕量Sc(III)的预富集，结果令人满意。
