A method for the preconcentration of trace heavy metal ions in environmental samples has been reported. The presented method is based on the sorption of Cu(II), Cd(II), Ni(II) and Cr(III) ions with salicylic acid as respective chelate on silica-coated magnetite nanoparticles. Prepared adsorbent was characterized by XRD, SEM, BET and FT-IR measurements. The metals content of the sorbed complexes are eluted using 4.0 mL of 1.0 mol L-1 nitric acid. The influences of the analytical parameters including pH, amount of solid phase and condition of eluting solution, the effects of matrix ions on the retention of the analytes were examined. The accuracy and precision of suggested method were tested by analyzing of certified reference materials. The detection limits (3Sb/m, N = 8) for Cu(II), Cd(II), Ni(II) and Cr(III) ions are 0.22, 0.11, 0.27 and 0.15 μg L-1, respectively, and the maximum preconcentration factor is 200. The method was successfully applied to the evaluation of these trace and toxic metals in various waters, foods and other samples.
The electrocatalytic oxidation of hydroxylamine was studied at the surface of a carbon paste electrode (CPE) spiked with multi-wall carbon nanotubes (MWCNT) and 4-hydroxy-2-(triphenylphosphonio)phenolate (HTP). The modified electrode (HTP-MWCNT-CPE) exhibits an excellent electrochemical catalytic activity toward hydroxylamine oxidation. The results show that there is a dramatic enhancement on the anodic peak current of hydroxylamine oxidation at the HTP-MWCNT-CPE in comparison the value obtained at HTP-CPE and MWCNT-CPE. The kinetic parameters of the electron transfer coefficient, a, the heterogeneous electron transfer rate constant, k 0 , and the exchange current density, j 0 , for oxidation of hydroxylamine at the HTP-MWCNT-CPE were determined using cyclic voltammetry. Differential pulse voltammetry exhibits three dynamic linear ranges of 2.0-10.0 mM, 10.0-1000.0 mM and 1000.0-8000.0 mM, and a lower detection limit of 0.16 mM for hydroxylamine. Finally, the modified electrode activity was studied for hydroxylamine determination in two water samples and satisfactory results were obtained.
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