Abstract

The rapid development in nanomaterials and nanotechnologies has provided many new opportunities in the area related to analytical chemistry. In this paper the unique properties of these materials were used in order to preconcentrate heavy metals prior to detection by spectroscopic techniques. A novel, simple and highly reliable method for the preconcentration of trace amounts of chromium, manganese, cobalt, nickel, copper and zinc using electrochemically assisted sorption on oxidized multiwalled carbon nanotubes (MWCNTs) is developed. The proposed method is based on the application of an electric field to support the sorption process on oxidized MWCNTs. The proposed method was used to preconcentrate trace elements from water of pH = 4. After the preconcentration process, oxidized MWCNTs were directly measured using an energy dispersive X-ray fluorescence (EDXRF) spectrometer that reduces the number of chemicals required and minimizes sample handling. Besides EDXRF, any spectroscopy technique allowing the measurement of solid samples can be applied. The various parameters including pH of the solution, amounts of oxidized MWCNTs, sample volume and the influence of voltage as well as the time of assisted electric field on the sorption process were investigated for the optimization of the analytical procedure. Under optimized conditions the proposed preconcentration method offers a high recovery of 99% (Cr), 97% (Mn), 94% (Co), 96% (Ni), 92% (Cu) and 93% (Zn) and good precision of sample preparation (RSD) within 3.5-7%. If measurements are performed using the EDXRF spectrometer, the detection limits are 1 ng mL(-1), 5 ng mL(-1), 5 ng mL(-1), 7 ng mL(-1), 1 ng mL(-1), 8 ng mL(-1) for Cr(III), Mn(II), Co(II), Ni(II), Cu(II) and Zn(II), respectively.

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