, and Ni 2+ ) do not interfere under the same conditions, due to the absence of oxidative activity of these ions, which guarantees the high selectivity of the proposed optical sensor towards Hg 2+ . The limits of detection and quantification were found to be 0.9 g L −1 and 2.7 g L −1 , respectively, and relative standard deviations varied in the range 9-12% for Hg content from 0.9 to 12.5 g L −1 and 5-9% for Hg levels from 25 to 500 g L −1 . The method was validated by analysis of CRM Estuarine Water BCR505. A possible mechanism of interaction between AgNPs and Hg 2+ for both concentration ranges was proposed on the basis of UV-Vis, TEM, and SAED analyses.
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.
Various types of nanomaterials such as magnetic nanoparticles, carbon nanostructures, metal oxides, noble metal nanoparticles, and ion imprinted polymers have been incorporated in new innovative approaches for speciation analysis.
A novel solution-solid synthesis method for preparation of ZnO and Au/ZnO composite nanocrystals using starch matrix has been developed and optimized. The process is characterized by simplicity, environmental compatibility and good performance. Nanocomposite samples with different gold content have been synthesized and studied with respect to their structure, size and shape of nanocrystals, thermal behavior, surface characteristics and optical properties, as well as their photocatalytic activity. We have found that modification of nanocrystalline ZnO with gold nanocrystals strongly influences the porosity of nanocomposites -less micro-and mesopores are formed, which results in a reduced specific surface area. The synthesized ZnO and Au/ZnO nanocrystals are active photocatalysts for the photocatalytic degradation of methylene blue (MB), as a model pollutant dye, in the UV region. There is a decrease in photocatalytic activity with an increase of the gold content in the nanocomposite photocatalyst. The degree of MB degradation obtained with a pure ZnO sample is comparable to that with the Au/ ZnO photocatalyst with the lowest gold content 0.05 at. %. New and interesting result has been obtained relating to maximum specific (intrinsic) photocatalytic activity of 0.05 at. % Au/ZnO nanocrystals.
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