Analytical Sciences

Use of Ni/Ni_xB Nanoparticles as a Novel Adsorbent for the Preconcentration of Mercury Species prior to Cold Vapor-Atomic Fluorescence Spectrometric Determination

Onur YAYAYÜRÜK and Emür HENDEN

Department of Chemistry, Faculty of Science, Ege University, Bornova, Izmir 35100, Turkey

A selective matrix separation/enrichment method, utilizing a simple batch procedure with nickel/nickel boride (Ni/Ni_xB) nanoparticles was proposed for the determination of inorganic mercury(II), Hg²⁺ and methyl mercury(I), CH₃Hg⁺ in waters prior to cold vapor-atomic fluorescence spectrometry (CV-AFS). The Ni/Ni_xB nanoparticles, were synthesized by the chemical reduction of Ni(II) to Ni/Ni_xB. The novel adsorbent was selective to Hg²⁺ and CH₃Hg⁺ species between pH values of 4 – 10. Both of the mercury species were recovered from the adsorbent using 1.0 mol L⁻¹ hot HNO₃ with high efficiency. It was observed that the adsorbent selectively removed Hg²⁺ and CH₃Hg⁺ from the bulk solution in the presence of several competitor ions (As³⁺, Sb³⁺, Pb²⁺, Zn²⁺, Cu²⁺, Cd²⁺ and Fe³⁺) with ≥96% adsorption. The limit of detection (3σ above blank) was found to be 1.8 ng L⁻¹ with a preconcentration factor of 20. The validation of the method was tested through spike recovery experiments with several water samples (tap and seawater) at μg L⁻¹ concentration levels, and all recovery values were found to vary between 95 and 105%.

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