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负载银纳米颗粒的亚微米级二氧化硅球作为地表水中无机汞的新型高效吸附剂

Submicron silica spheres decorated with silver nanoparticles as a new effective sorbent for inorganic mercury in surface waters.

作者信息

Yordanova Tanya, Vasileva Penka, Karadjova Irina, Nihtianova Diana

机构信息

Department of Analytical Chemistry, Faculty of Chemistry and Pharmacy, University of Sofia, Bulgaria.

出版信息

Analyst. 2014 Mar 21;139(6):1532-40. doi: 10.1039/c3an01279d.

Abstract

An analytical method using silica supported silver nanoparticles as a novel sorbent for the enrichment and determination of inorganic mercury (iHg) in surface water samples has been developed. Silver nanoparticles (AgNPs) were synthesized by a completely green procedure and were deposited onto the amine functionalized surface of silica submicrospheres (SiO2-NH2). The prepared nanocomposite material (SiO2/AgNPs) was characterized by transmission electron microscopy, UV-vis spectroscopy, X-ray diffraction and atomic force microscopy. The sorption and desorption characteristics of the nanosorbent SiO2/AgNPs toward Hg species were investigated by a batch method. An excellent separation of iHg and methylHg was achieved in 20 minutes at pH 2. The high selectivity of the SiO2/AgNPs toward iHg was explained by Hg(ii) reduction and subsequent silver-mercury amalgam formation. The analytical procedure for the enrichment and determination of inorganic mercury in surface waters was developed based on solid phase extraction and ICP-MS measurements. The total Hg content was determined after water sample mineralization. The recoveries reached for iHg in different surface waters e.g. river and Black sea water samples varied from 96-101%. The limits of quantification are 0.002 μg L(-1) and 0.004 μg L(-1) for iHg and total Hg, respectively; the relative standard deviations varied in the ranges of 5-9% and 6-11% for iHg and total Hg, respectively, for Hg content from 0.005 to 0.2 μg L(-1). The accuracy of the procedure developed for total Hg determination was confirmed by a comparative analysis of surface river (ICP-MS) and sea (CV AFS) waters.

摘要

已开发出一种分析方法,该方法使用二氧化硅负载的银纳米颗粒作为新型吸附剂,用于富集和测定地表水样品中的无机汞(iHg)。银纳米颗粒(AgNPs)通过完全绿色的方法合成,并沉积在二氧化硅亚微球(SiO₂-NH₂)的胺官能化表面上。通过透射电子显微镜、紫外-可见光谱、X射线衍射和原子力显微镜对制备的纳米复合材料(SiO₂/AgNPs)进行了表征。采用分批法研究了纳米吸附剂SiO₂/AgNPs对汞物种的吸附和解吸特性。在pH 2条件下,20分钟内实现了iHg和甲基汞的良好分离。SiO₂/AgNPs对iHg的高选择性是由Hg(ii)还原及随后形成银汞合金来解释的。基于固相萃取和电感耦合等离子体质谱测量,开发了地表水无机汞富集和测定的分析程序。水样矿化后测定总汞含量。不同地表水(如河水和黑海海水样品)中iHg的回收率在96%-101%之间。iHg和总汞的定量限分别为0.002 μg L⁻¹和0.004 μg L⁻¹;对于0.005至0.2 μg L⁻¹的汞含量,iHg和总汞的相对标准偏差分别在5%-9%和6%-11%范围内。通过对地表河流(电感耦合等离子体质谱)和海水(冷原子荧光光谱法)的对比分析,证实了所开发的总汞测定程序的准确性。

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