Bravo-Sánchez L R, de la Riva B S, Costa-Fernández J M, Pereiro R, Sanz-Medel A
Department of Physical and Analytical Chemistry, Faculty of Chemistry, University of Oviedo, Julián Claveria, 8, 33006, Oviedo, Spain.
Talanta. 2001 Dec 24;55(6):1071-8. doi: 10.1016/s0039-9140(01)00523-9.
The capabilities of three solid chelating reagents were compared for the preconcentration of lead and mercury in high salinity aqueous samples (sea waters). The tested materials were 7-(4-ethyl-1-methyloctyl)-8-hydroxiquinoline (Kelex 100) adsorbed on Bondapack C18 (Kelex-100/C18), 8-hydroxiquinoline immobilized on vinyl co-polymer Toyopearl gel (TSK) and the commercial polystyrene/DVB ion exchange resin with paired iminodiacetate groups (Chelex-100). The two metals preconcentration and final determination were carried out in a flow injection system, coupled on-line to an atomic absorption spectrometric detector. Analytes were preconcentrated in the minicolumn, packed with the materials under investigation, while elution was achieved by injection of 500 mul of an adequate mineral acid solution. The different packing materials and minicolumn designs have been evaluated in terms of sensitivity for simultaneous preconcentration of both metals in sea water. Regarding the solid support, the best results were obtained for the TSK solid phase. Concerning the minicolumn design, the behavior was different for lead and mercury. Lead was quantitatively eluted with 0.5 M HCl and best performance was achieved when packing the solid material in a minicolumn with relatively small volume (1 cm length and 2.5 mm i.d.). In the case of mercury, bigger minicolumn volumes (5.5 cm length and 5.0 mm i.d.) and mixtures, 2 M HCl+1 M HNO(3), were required for its quantitative recovery and elution. The system has been evaluated for quantitative determination of the two metals under study in different Asturian coastal aqueous samples.
比较了三种固体螯合试剂对高盐度水样(海水)中铅和汞的预富集能力。测试材料包括吸附在Bondapack C18上的7-(4-乙基-1-甲基辛基)-8-羟基喹啉(Kelex 100)(Kelex-100/C18)、固定在乙烯基共聚物Toyopearl凝胶上的8-羟基喹啉(TSK)以及带有成对亚氨基二乙酸基团的商用聚苯乙烯/二乙烯基苯离子交换树脂(Chelex-100)。两种金属的预富集和最终测定在流动注射系统中进行,并与原子吸收光谱检测器在线联用。分析物在填充有待研究材料的微型柱中进行预富集,通过注入500 μl适当的无机酸溶液实现洗脱。根据对海水中两种金属同时预富集的灵敏度,对不同的填充材料和微型柱设计进行了评估。就固体载体而言,TSK固相获得了最佳结果。关于微型柱设计,铅和汞的行为有所不同。用0.5 M HCl可将铅定量洗脱,当将固体材料填充到体积相对较小(长度1 cm,内径2.5 mm)的微型柱中时,性能最佳。对于汞,需要更大体积的微型柱(长度5.5 cm,内径5.0 mm)以及2 M HCl + 1 M HNO₃的混合溶液才能实现其定量回收和洗脱。该系统已用于对不同阿斯图里亚斯沿海水样中所研究的两种金属进行定量测定。