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Functionalized nanometer-sized alumina supported micro-solid phase extraction coupled to inductively coupled plasma mass spectrometry for preconcentration and determination of trace metal ions in gasoline samples

机译:功能化的纳米级氧化铝支持的微固相萃取与电感耦合等离子体质谱联用,用于汽油样品中的痕量金属离子的预浓缩和测定

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摘要

Nanometer-sized alumina functionalized with [3-(2-aminoethylamino) propyl] trimethoxysilane (nano-Al2O3/AAPTMS) was prepared as an adsorbent for preconcentration of trace element ions in gasoline samples. The nano-Al2O3 was characterized by XRD, SEM and BET techniques and the functionalized adsorbent was characterized by ATR-FTIR spectroscopy. The nano-Al2O3/AAPTMS sorbent was used as the packing material in the supported micro-solid-phase extraction (mu-SPE) device. The latter was coupled with inductively coupled plasma mass spectrometry (ICP-MS) for preconcentration and determination of trace elements in gasoline samples. The optimization of the preconcentration system was achieved by a multivariate strategy. Under optimized conditions, limits of detection (LOD) and quantification (LOQ) ranged from 0.2-0.7 ng L-1 to 0.7-2.3 ng L-1, respectively, and a preconcentration factor of 40 was achieved. The validity of the developed mu-SPE-ICP-MS procedure was confirmed by analysis of spiked gasoline samples. The supported mu-SPE-ICP-MS method was applied for quantification of Co, Cr, Mn, Ni and Ti in commercial gasoline samples. The mu SPE device coupled with ICP-MS provided improved LOD and LOQ for trace metal analysis in a gasoline matrix and significantly reduced matrix interference.
机译:制备了用[3-(2-氨基乙基氨基)丙基]三甲氧基硅烷官能化的纳米级氧化铝(纳米Al2O3 / AAPTMS)作为吸附剂,用于对汽油样品中的痕量离子进行预浓缩。通过XRD,SEM和BET技术对纳米Al2O3进行了表征,并通过ATR-FTIR光谱对了功能化吸附剂进行了表征。纳米Al2O3 / AAPTMS吸附剂被用作支持的微固相萃取(mu-SPE)设备中的填充材料。后者与电感耦合等离子体质谱法(ICP-MS)结合使用,可对汽油样品中的痕量元素进行预富集和测定。预浓缩系统的优化是通过多变量策略实现的。在最佳条件下,检出限(LOD)和定量限(LOQ)分别在0.2-0.7 ng L-1至0.7-2.3 ng L-1范围内,预浓缩系数达到40。通过分析加标汽油样品,证实了开发的mu-SPE-ICP-MS方法的有效性。支持的mu-SPE-ICP-MS方法用于定量商业汽油样品中的Co,Cr,Mn,Ni和Ti。 mu SPE装置与ICP-MS结合使用,可改善汽油基质中痕量金属的LOD和LOQ,并显着降低了基质干扰。

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