Zhang Nan, Hu Bin, Huang Chaozhang
Department of Chemistry, Wuhan University, Wuhan 430072, PR China.
Anal Chim Acta. 2007 Jul 30;597(1):12-8. doi: 10.1016/j.aca.2007.06.045. Epub 2007 Jun 28.
Dysprosium(III)-imprinted thenoyltrifluoroacetone (TTA) modified silica gel sorbent was synthesized by surface imprinting technique and was employed as a selective solid-phase extraction material for flow injection solid-phase extraction on-line coupled with inductively coupled plasma-atomic emission spectrometry (ICP-AES) determination of Dy(III). The largest selectivity coefficient for Dy(III) in the presence of competitive ions such as La(III), Nd(III) and Gd(III) was above 350. The static adsorption capacity and selectivity coefficient of the imprinted sorbent are higher than those of the non-imprinted sorbent and the imprinted TTA modified silica gel sorbent offered a fast kinetics for the adsorption and desorption of Dy(III). With a sample loading flow rate of 2.5 mL min(-1) for 48 s preconcentration and elution flow rate of 1.5 mL min(-1) for 8 s elution, an enrichment factor of 10 and the sample frequency of 40 sample h(-1) were obtained. Detection limits (3sigma) based on three times standard deviations of the blanks by eight replicates was 0.2 ng mL(-1) and the precisions (R.S.D.s) was 1.5% (n=8, c=40 ng mL(-1)). To validate the proposed method, two certified reference materials of GBW07401 soil and GBW07301a sediment were analyzed and the determined values were in a good agreement with the certified values. The method is rapid, selective, sensitive and applicable to the determination of trace Dy(III) in environmental samples with complicated matrix.
采用表面印迹技术合成了镝(III)印迹的噻吩甲酰三氟丙酮(TTA)修饰硅胶吸附剂,并将其用作流动注射固相萃取的选择性固相萃取材料,在线联用电感耦合等离子体原子发射光谱法(ICP-AES)测定镝(III)。在La(III)、Nd(III)和Gd(III)等竞争离子存在下,镝(III)的最大选择性系数高于350。印迹吸附剂的静态吸附容量和选择性系数高于非印迹吸附剂,且印迹TTA修饰硅胶吸附剂对镝(III)的吸附和解吸具有快速动力学。进样流速为2.5 mL min⁻¹,进样48 s进行预富集,洗脱流速为1.5 mL min⁻¹,洗脱8 s,富集倍数为10,进样频率为40次/h。基于8次重复测定空白值3倍标准偏差的检出限为0.2 ng mL⁻¹,精密度(相对标准偏差)为1.5%(n = 8,c = 40 ng mL⁻¹)。为验证该方法,分析了GBW07401土壤和GBW07301a沉积物两种有证标准物质,测定值与认定值吻合良好。该方法快速、选择性好、灵敏度高,适用于复杂基体环境样品中痕量镝(III)的测定。