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Macroemulsion-based dispersive magnetic solid phase extraction for preconcentration and determination of copper(II) in gasoline
Microchimica Acta ( IF 5.7 ) Pub Date : 2018-01-10 , DOI: 10.1007/s00604-017-2634-0
Francisco Antônio S. Cunha , Danilo Tadeu S. Ferreira , Willy C. R. Andrade , Julys Pablo A. Fernandes , Wellington S. Lyra , Amália G. G. Pessoa , Mario Cesar Ugulino de Araujo

AbstractA new method referred to as microemulsion-based Dispersive Magnetic Solid-Phase Extraction (MDM-SPE) is presented for use in the extraction and preconcentration of metal ions from complex organic matrices. MDM-SPE combines the features of magnetic nanoparticles (MNPs) and microemulsions. It was successfully applied to the extraction of copper(II) from gasoline prior to its determination by Graphite Furnace Atomic Absorption Spectrometry (GF-AAS). The material for use in MDM-SPE was obtained by first functionalizing MNPs of the type Fe3O4@Al2O3 with sodium dodecyl sulfate and the chelator 1-(2-pyridylazo)-2-naphthol (PAN) dispersed in 1-propanol. The resulting functionalized magnetic MNPs were dispersed in a microemulsion prepared from gasoline, buffer, and 1-propanol. After waiting for 5 s (during which the formation of the copper complex on the MNPs is complete), the MNPs are magnetically separated. The complex was then eluted with 2 mol L−1 HNO3, and the eluate submitted to GF-AAS. Various parameters were optimized. Copper(II) can be quantified by this method over a linear range that extends from 2.0 to 10.0 μg·L−1. Other figures of merit include (a) a 37 ng·L−1 detection limit, (b) a repeatability of 1.1%, (c) a reproducibility of 2.1%, and (d) an enrichment factor of nine. The high surface-to-volume ratio of the microemulsion containing the dispersed magnetic sorbent warrants an efficient contact for reaction between copper(II) and the complexing agent, and this results in fast (about 40 s) extraction and pre-concentration of copper(II). MDM-SPE is accurate, precise and efficient. Microemulsions do not break down, and phase separation, heating, laborious, and time-consuming sample preparation, and incorporation of impurities into the graphite furnace (which can generate inaccuracies in GF-AAS analysis) are not needed. Graphical abstractSchematic of a new method for Microemulsion-based Dispersive Magnetic Solid-Phase Extraction (MDMSPE) using functionalized magnetic nanoparticles (FMNPs). It was applied to the preconcentration of copper(II) in gasoline.

中文翻译:

基于粗乳液的分散磁固相萃取预浓缩和测定汽油中的铜 (II)

摘要 提出了一种称为基于微乳液的分散磁性固相萃取 (MDM-SPE) 的新方法,用于从复杂有机基质中萃取和预浓缩金属离子。MDM-SPE 结合了磁性纳米粒子 (MNP) 和微乳液的特性。在通过石墨炉原子吸收光谱法 (GF-AAS) 测定之前,它已成功应用于从汽油中提取铜 (II)。用于 MDM-SPE 的材料是通过首先用十二烷基硫酸钠和分散在 1-丙醇中的螯合剂 1-(2-吡啶偶氮)-2-萘酚 (PAN) 对 Fe3O4@Al2O3 类型的 MNP 进行功能化而获得的。所得官能化磁性 MNP 分散在由汽油、缓冲液和 1-丙醇制备的微乳液中。等待 5 秒后(在此期间 MNP 上的铜配合物形成完成),MNP 被磁分离。然后用 2 mol L-1 HNO3 洗脱复合物,并将洗脱液送至 GF-AAS。优化了各种参数。铜 (II) 可以通过该方法在 2.0 至 10.0 μg·L-1 的线性范围内定量。其他优点包括 (a) 37 ng·L-1 检测限,(b) 1.1% 的重复性,(c) 2.1% 的再现性,以及 (d) 9 的富集因子。含有分散磁性吸附剂的微乳液的高表面积与体积比保证了铜 (II) 与络合剂之间的反应有效接触,这导致快速(约 40 秒)提取和预浓缩铜(二)。MDM-SPE 准确、精确且高效。微乳液不会分解,并且不需要相分离、加热、费力且耗时的样品制备以及将杂质掺入石墨炉(这会导致 GF-AAS 分析不准确)。图形摘要使用功能化磁性纳米粒子 (FMNP) 进行基于微乳液的分散磁性固相萃取 (MDMSPE) 的新方法示意图。应用于汽油中铜(II)的预浓缩。图形摘要使用功能化磁性纳米粒子 (FMNP) 进行基于微乳液的分散磁性固相萃取 (MDMSPE) 的新方法示意图。应用于汽油中铜(II)的预浓缩。图形摘要使用功能化磁性纳米粒子 (FMNP) 进行基于微乳液的分散磁性固相萃取 (MDMSPE) 的新方法示意图。应用于汽油中铜(II)的预浓缩。
更新日期:2018-01-10
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