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烯丙基硫脲功能化磁性吸附剂用于原子吸收光谱法测定镉、铜和铅离子之前的萃取。

Allylthiourea functionalized magnetic adsorbent for the extraction of cadmium, copper and lead ions prior to their determination by atomic absorption spectrometry.

机构信息

State Key Laboratory of Marine Environmental Science; Key Laboratory of the Ministry of Education for Coastal and Wetland Ecosystems; Center for Marine Environmental Chemistry and Toxicology, College of the Environment and Ecology, Xiamen University, P. O. Box 1009, Xiamen, 361005, China.

出版信息

Mikrochim Acta. 2019 Jan 7;186(2):51. doi: 10.1007/s00604-018-3101-2.

Abstract

A quick and sensitive method was developed for the trace determination of Cd(II), Pb(II) and Cu(II) ions in water and bean samples. It is based on a combination of magnetic solid phase extraction (MSPE) and graphite furnace atomic absorption spectrometry (GFAAS). Allylthiourea (which contains abundant sulfur and nitrogen atoms) was copolymerized with ethylene dimethacrylate on the surface of magnetite (FeO) nanoparticles to prepare a new adsorbent for use in MSPE. Various technologies were used to characterize the morphology, spectroscopic and magnetic properties of the adsorbent, and several parameters that affect the extraction performance were optimized. The adsorbent can enrich Cd(II), Pb(II) and Cu(II) ions via chelation interaction. Following elution with 0.1 mol·L HNO, the ions were quantified by GFAAS. Under the most favorable conditions, the limits of detection are from 3.3-7.2 ng·L for water samples, and 1.1-1.5 μg·kg for beans. The method displays wide linear analytical ranges and good precision. It was successfully applied to the determination of the metal ions in water and bean samples. The recoveries from spiked samples ranged between 80.5 and 114% in water, and from 82.2 to 118% in bean samples. The relative standard deviations of reproducibility were < 10%. Graphical abstract Schematic presentation of the magetic solid phase extraction (MSPE) for the analysis of Cd(II), Pb(II) and Cu(II). MNP: magnetic nanoparticles; ATED: allylthiourea ethylene dimethacrylate copolymer.

摘要

一种快速灵敏的方法被开发用于痕量测定水中和豆类样品中的 Cd(II)、Pb(II) 和 Cu(II) 离子。它基于磁固相萃取 (MSPE) 和石墨炉原子吸收光谱 (GFAAS) 的结合。烯丙基硫脲(含有丰富的硫和氮原子)与二乙烯基苯共聚在磁铁矿 (FeO) 纳米粒子的表面上,制备用于 MSPE 的新型吸附剂。采用多种技术对吸附剂的形貌、光谱和磁性进行了表征,并对影响萃取性能的几个参数进行了优化。该吸附剂通过螯合作用富集 Cd(II)、Pb(II) 和 Cu(II) 离子。用 0.1 mol·L HNO 洗脱后,用 GFAAS 定量测定离子。在最有利的条件下,水样品的检测限为 3.3-7.2 ng·L,豆类样品的检测限为 1.1-1.5 μg·kg。该方法具有较宽的线性分析范围和良好的精密度。成功应用于水和豆类样品中金属离子的测定。加标样品的回收率在水中为 80.5-114%,在豆类样品中为 82.2-118%。重现性的相对标准偏差<10%。

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