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Ultra-trace tellurium preconcentration and speciation analysis in environmental samples with a novel magnetic polymeric ionic liquid nanocomposite and magnetic dispersive micro-solid phase extraction with flow-injection hydride generation atomic fluorescence spectrometry detection
Spectrochimica Acta Part B: Atomic Spectroscopy ( IF 3.3 ) Pub Date : 2019-12-01 , DOI: 10.1016/j.sab.2019.105705
Mauricio Llaver , Francisco A. Casado-Carmona , Rafael Lucena , Soledad Cárdenas , Rodolfo G. Wuilloud

Abstract A highly efficient magnetic dispersive micro-solid phase extraction (M-D-μSPE) method was developed for Te preconcentration and speciation analysis in different environmental samples. A novel magnetic polymeric ionic liquid nanocomposite synthesized based on the Radziszewski reaction was applied for the selective retention of Te(IV) species, followed by elution with 5 mol L−1 HCl and determination by flow-injection hydride generation atomic fluorescence spectrometry. Te(VI) was selectively determined by difference between total Te and Te(IV) after a pre-reduction step. Studies on the sorption capacity of the nanocomposite were performed, while several parameters concerning the retention, separation and elution were optimized. A 100% retention efficiency and a sensitivity enhancement factor of 67 were achieved. Limits of detection of 1.9 ng L−1 and 3.7 ng L−1, and standard deviations of 4.3% and 5.1% were obtained for Te(IV) and Te(VI). A gas-liquid separator with a low dead volume was used for reduced dispersion of the flow injection signals and additional sensitivity enhancement. Finally, the feasibility of the proposed M-D-μSPE method for Te speciation was demonstrated by the analysis of several environmental samples, such as tap, rain, river and underground waters, soils and sediments, with excellent recovery results in spiked samples.

中文翻译:

使用新型磁性聚合物离子液体纳米复合材料和磁分散微固相萃取与流动注射氢化物发生原子荧光光谱法检测环境样品中的超痕量碲预富集和形态分析

摘要 开发了一种高效的磁分散微固相萃取 (MD-μSPE) 方法,用于不同环境样品中 Te 的富集和形态分析。基于 Radziszewski 反应合成的新型磁性聚合物离子液体纳米复合材料用于选择性保留 Te(IV) 物种,然后用 5 mol L-1 HCl 洗脱并通过流动注射氢化物发生原子荧光光谱法测定。在预还原步骤后,Te(VI) 通过总 Te 和 Te(IV) 之间的差异选择性地确定。对纳米复合材料的吸附能力进行了研究,同时优化了有关保留、分离和洗脱的几个参数。实现了 100% 的保留效率和 67 的灵敏度增强因子。检测限 1。对于 Te(IV) 和 Te(VI),获得了 9 ng L-1 和 3.7 ng L-1,以及 4.3% 和 5.1% 的标准偏差。具有低死体积的气液分离器用于减少流动注射信号的分散和额外的灵敏度增强。最后,通过对自来水、雨水、河流和地下水、土壤和沉积物等几种环境样品的分析,证明了所提出的 MD-μSPE 方法对 Te 形态形成的可行性,在加标样品中具有出色的回收率。
更新日期:2019-12-01
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