Yordanova Tanya, Vasileva Penka, Karadjova Irina, Nihtianova Diana
Department of Analytical Chemistry, Faculty of Chemistry and Pharmacy, University of Sofia, Bulgaria.
Analyst. 2014 Mar 21;139(6):1532-40. doi: 10.1039/c3an01279d.
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.
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。