Laboratory of Analytical Chemistry, Department of Chemistry, Faculty of Science, Aristotle University, 54124 Thessaloniki, Greece.
Talanta. 2013 Jun 15;110:229-35. doi: 10.1016/j.talanta.2013.02.035. Epub 2013 Feb 22.
A new automatic sequential injection (SI) system for on-line magnetic sorbent extraction coupled with electrothermal atomic absorption spectrometry (ETAAS) has been successfully developed for metal determination. In this work, we reported effective on-line immobilization of magnetic silica particles into a microcolumn by the external force of two strong neodymium iron boron (NdFeB) magnets across it, avoiding the use of frits. Octadecylsilane functionalized maghemite magnetic particles were used as sorbent material. The potentials of the system were demonstrated for trace cadmium determination in water samples. The method was based on the on-line complex formation with diethyldithiocarbamate (DDTC), retention of Cd-DDTC on the surface of the MPs and elution with isobutyl methyl ketone (IBMK). The formation mechanism of the magnetic solid phase packed column and all critical parameters (chemical, flow, graphite furnace) influencing the performance of the system were optimized and offered good analytical characteristics. For 5 mL sample volume, a detection limit of 3 ng L(-1), a relative standard deviation of 3.9% at 50 ng L(-1) level (n=11) and a linear range of 9-350 ng L(-1) were obtained. The column remained stable for more than 600 cycles keeping the cost down in routine analysis. The proposed method was evaluated by analyzing certified reference materials and natural waters.
一种新的自动顺序注射(SI)系统已成功开发用于在线磁固相萃取与电热原子吸收光谱(ETAAS)联用,用于金属测定。在这项工作中,我们报道了通过两个强钕铁硼(NdFeB)磁铁对微柱施加的外力将磁性硅胶颗粒有效在线固定在微柱内,避免了使用烧结片。十八烷基硅烷功能化磁赤铁矿磁性颗粒被用作吸附材料。该方法基于与二乙基二硫代氨基甲酸盐(DDTC)的在线络合,Cd-DDTC 在 MPs 表面的保留和异丁基甲基酮(IBMK)的洗脱。优化了磁性固相聚相填充柱的形成机制和所有影响系统性能的关键参数(化学、流动、石墨炉),并提供了良好的分析特性。对于 5 mL 样品体积,检测限为 3 ng L(-1),50 ng L(-1) 水平时的相对标准偏差为 3.9%(n=11),线性范围为 9-350 ng L(-1)。该柱在 600 次以上的循环中保持稳定,降低了常规分析的成本。通过分析认证参考材料和天然水来评估所提出的方法。