A simple and eco-friendly electrochemical sensor for the anti-inflammatory diclofenac (DIC) was developed in a chitosan nanocomposite carbon paste electrode (M-Chs NC/CPE). The M-Chs NC/CPE was characterized with FTIR, XRD, SEM, and TEM for the size, surface area, and morphology. The produced electrode showed a high electrocatalytic activity to use the DIC in 0.1 M of the BR buffer (pH 3.0). The effect of scanning speed and pH on the DIC oxidation peak suggests that the DIC electrode process has a typical diffusion characteristic with two electrons and two protons. Furthermore, the peak current linearly proportional to the DIC concentration ranged from 0.025 M to 4.0 M with the correlation coefficient (r2). The sensitivity, limit of detection (LOD; 3σ), and the limit of quantification (LOQ; 10σ) were 0.993, 9.6 µA/µM cm2, 0.007 µM, and 0.024 µM, respectively. In the end, the proposed sensor enables the reliable and sensitive detection of DIC in biological and pharmaceutical samples.
The aqueous basic systems NiSO4·6H2O/K2S2O8 (pH = 14) and NiSO4·6H2O/KBrO3 (pH = 11.5) were investigated for the catalytic conversion of benzyl alcohol and some para-substituted benzyl alcohols to their corresponding acids in 75–97% yields at room temperature. The active species was isolated and characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray powder diffraction, EDX and FT-IR techniques, and identified as comprising NiO2 nanoparticles (NPNPs). The SEM and TEM images of the Ni peroxide samples showed a fine spherical-like aggregation of NiO2 molecules with a nearly homogeneous partial size and confirmed the aggregation’s size to be in the range of 2–3 nm. The yields, turn over (TO) and turn over frequencies (TOF) were calculated. It was noticed that the aromatic alcohols containing para-substituted electron donation groups gave better yields than those having electron withdrawing groups. The optimum conditions for this catalytic reaction were studied using benzyl alcohol as a model. The mechanism of the catalytic conversion reaction was suggested, in which the produced NPNPs convert alcohols to acids in two steps through the formation of the corresponding aldehyde. The produced NiO because of this conversion is converted again to NPNPs by the excess of K2S2O8 or KBrO3. This catalytic cycle continues until all of the substrate is oxidized.
In the present work; the impact of the solar and electrical energy on microstructures, crystalline phases and mechanical properties in the binary aluminum borate/alumina ceramic composite, prepared by wet method were studied. Solar and electrical energy were employed by sintering the prepared samples at 1400 °C then thermally shocked at 1200 °C and 1000 °C in the 100 and 20 cycles respectively. Corundum (Al2O3) with a low content of aluminum borate (Al18B4O33) was developed after sintering process and thermal shock. The scanning electron microscopy indicated a partial melting since the nano-scale rod crystals edges changed into curved one. Mechanical properties comprising (Young´s (E) and Coulomb´s (G) elastic moduli of elasticity) and density were investigated. The mechanical properties of these materials were deteriorated when compared with pure alumina ceramics. The flexural strength values of alumina ceramic showed the highest value of 244 MPa compared to 67 MPa for alumina/aluminum borate composite, after 100 cycles of thermal shock.