Nickel and cobalt sulfides are promising materials in different cutting-edge research areas like solar cells, supercapacitors, catalysts, and electrode materials. Nickel and cobalt sulfides with various stoichiometries have been synthesized sonochemically from Ni(CH3COO)2 ∙ 4H2O, Co(CH3COO)2 ∙ 2H2O and different sulfur precursors using a direct immersion ultrasonic probe. The products were characterized by X-ray powder diffraction, transmission electron microscopy (TEM) including EDX analysis, IR and UV–Vis spectroscopy and elemental analysis. Following products have been obtained: NiS, Ni3S4, CoS1.097 and Co9S8, with average crystallite sizes in the range 7−30 nm. Effects of different reaction conditions on the size, morphology and optical band-gap energy were evaluated. Optical band-gap energies in the range 3.3 eV−3.8 eV were observed for the obtained nanoparticles.
Chromium, cadmium and lead were determined in different fractions of the winemaking process such as in grape, pressed pomace, must deposit, deposit of lees, must and wine. Grape, pressed pomace, must deposit and deposit of lees were digested by a high-pressure microwave-assisted digestion system with a mixture of nitric acid and hydrogen peroxide, while for must and wine no special treatment was required. The temperature programs of the graphite furnace were optimised and different matrix modifiers were applied: Mg(NO3)2, NaVO3 for Cr and NH4H2PO4, Pd(NO3)2 for Pb and Cd determinations. Mg(NO3)2 and NaVO3 thermally stabilized Cr and enabled the increase of pyrolysis temperatures up to 1500 degrees C. NH4H2PO4 and Pd(NO3)2 are suitable modifiers for Pb and allowed pyrolysis temperatures up to 800 degrees C in grape, pressed pomace and wine samples, 1100 degrees C in must samples and 1200 degrees C in deposit of lees. The non-specific background absorption of NH4H2PO4 was 1.5-2 orders of magnitude higher than that of the Pd(NO3)2.
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