Catalysts were synthesized with Ni and bentonite clay, without previous treatment, through wet impregnation with 5, 10 and 20% of Ni (m/m). They were characterized by energy dispersive X-ray fluorescence spectrometry (EDX), X-ray diffraction (XRD), temperature-programmed reduction (TPR), thermogravimetric analysis (TGA), adsorption and desorption of N2 at 77 K, and transmission electron microscopy (TEM). The catalytic activity in relation to the methane conversion reaction was evaluated at 500 ºC for 0.5 h. The addition of 10 and 20% of nickel to the clay led to a disordered bentonite structure, characterized by the disappearance of the 001 reflection on the X-ray diffractograms, with a consequent increase in the interaction between nickel oxide and clay (TPR). All catalysts synthesized showed catalytic activity in relation to the conversion of methane to form ordered carbon. The catalyst with 20% of nickel had the highest activity, with 74% of methane conversion.

Two different gold-silica-based nanomaterials were prepared: (i) silica-supported gold nanoparticles (AuNP/SiO2); and (ii) gold-silica core-shell nanoparticles (AuNP@SiO2). Three strategies for sample treatment (S), consisting in acid treatments, were employed: (S1) HNO3; (S2) HNO3 + HCl; and (S3) HF + HNO3 + HCl, applying microwave oven digestion for S2 and S3. From three calibration curves, slope, intercept, and linear correlation coefficient were obtained. The accuracy of the methods was evaluated by comparing the gold contents in a sample determined by flame atomic absorption spectrometry (FAAS) and by inductively coupled plasma atomic emission spectrometry (ICP-OES). Finally, the amount of gold for all samples was determined by FAAS. UV-Vis spectroscopy and transmission electron microscopy (TEM) were used to compare the material before and after sample treatment. By comparison, the application of S2 and S3 allowed the presence of gold on or in the silica matrix to be determined and the amount quantified.

The optimized analytical methodology described herein is based on an ion exchange column and an H3PO4 solution (pH 2.24) as the mobile phase, with a flow rate of 0.4 mL min-1 and refractive index detection (RID). On applying the methodology, it was possible to identify 7 products obtained from the oxidation of glycerol with an analysis time of 27 min. The developed method was validated through the evaluation of a series of analytical parameters. The results obtained were evaluated considering the peak area and peak height. The analytical curves showed a correlation coefficient of ≥ 0.986. The coefficient of variation values obtained were ≤ 3.60% for instrumental precision, ≤ 19.36% for intermediate precision in LOQ (1.25 µg mL-1) and ≤ 17.93% for repeatability in LOQ (1.25 µg mL-1) and different days. The limit of quantification established for all compounds was 1.25 µg mL-1 obtained through the parameters of the analytical curve. The accuracy of the method showed recovery values of 85.6 to 112.3% for real fortified sample at 3 concentration levels. Two different samples of glycerol oxidation products were applied to the validated methodology; one obtained from AuNP/SiO2 as catalyst (conversion of 62.42%), and other using AuNP/MWCNT (conversion of 89.5%).