Copper (II) oxide nanoparticles (CuONPs) were green synthesized using Ocimum basilicum leaves aqueous extract in which polyphenols act as reducing and stabilizing agents. The synthesized CuONPs were characterized using X-ray diffraction spectroscopy, Fourier transform infrared spectroscopy, transmission electron microscopy, selected area electron diffraction, and Brunauer–Emmett–Teller (BET) surface area analysis. The analyses indicated the formation of crystalline rod-like monoclinic pure CuONPs with a mean grain size of 15 nm, a surface area of 396 m2 g−1, and a total pore volume of 0.71 cm3 g−1. A glassy carbon electrode (GCE) was modified using the synthesized CuONPs and electropolymerized poly(methyl orange) (PMO). The modified PMO/CuONPs/GCE electrode was electrochemically characterized and applied for the estimation of folic acid (FA) by cyclic voltammetry, chronoamperometry, linear sweep voltammetry, and differential pulse voltammetry techniques. The influence of pH (7), scan rate (50 mV/s), supporting electrolyte (0.1 M KCl) and FA concentration has been optimized. FA is precisely determined in the range from 0.01 to 1.5 µΜ with a low detection limit (0.002 µΜ), a low quantitation limit (0.068 µΜ), high reproducibility (RSD 0.37, 10 measurements), and high stability (98% activity after 50 days). FA in food samples was determined by the new sensor with high recoveries from 93 to 108.8%.Graphical

Green analytical procedures are gaining popularity in the pharmaceutical research area as a way to reduce environmental impact and improve analyst health safety. The current work presents a green and sensitive electrochemical carbon paste electrode that has been chemically modified with zirconium dioxide and multi-walled carbon nanotubes for estimation of pyridoxine HCl (PYR) and doxylamine succinate (DOX) using the square wave voltammetric technique. Under optimum conditions, the linearity ranges were 20.00–2000.00 ng mL−1 and 2.00–20.00 µg mL−1 for both drugs in the 1st linear segment and 2nd linear segment, respectively. Stability testing assesses how the quality of a drug substance changes over time, depending on environmental and laboratory factors. DOX was found to undergo oxidative degradation when refluxed for 7 h using 30% H2O2 and the degraded product (DOX DEG) (toxic metabolite) was successfully characterized utilizing LC–MS. The developed electrode showed selectivity for the determination of binary mixture in pure form, pharmaceutical form, and in the presence of DOX DEG and common interfering molecules with good recovery. The proposed method was found to be eco-friendlier than the reported method in terms of the use of hazardous chemicals and solvents, energy consumption, and waste generation.Graphical

Three molecular catalysts based on mononuclear nickel(II) complexes with square planar geometries, [BzPy]2[Ni(mnt)2] (1), [BzPy]2[Ni(i-mnt)2] (2), and [BzPy]2[Ni(tdas)2] (3) (BzPy = benzyl pyridinium) are synthesized by the reaction of NiCl2∙6H2O, [BzPy]Br, and Na2(mnt)/Na2(i-mnt)/Na2(tdas) (mnt = 1,2-dicyanoethylene-1,2-dithiolate for (1), i-mnt = 2,2-dicyanoethylene-1,1-dithiolate for (2), and tdas = 1,2,5-thiadiazole-3,4-dithiolate for (3)), respectively. The structures and compositions of these three catalysts are characterized by XRD, elemental analysis, FT-IR, and ESI-MS. The electrochemical properties and the corresponding catalytic activities of these three catalysts are studied by cyclic voltammetry. The controlled-potential electrolysis with gas chromatography analysis confirms the hydrogen production with a turnover frequency (TOF) of 116.89, 165.51, and 189.16 moles of H2 per mole of catalyst per hour at a potential of − 0.99 V (versus SHE) in acetonitrile solutions containing the catalysts, respectively. In a neutral buffer solution, these three molecular catalysts exhibit a TOF of 411.85, 488.76, and 555.06 mol of H2 per mole of catalyst per hour at a potential of − 0.49 V (versus SHE), respectively, indicating that Complex 3 constitutes the better active catalyst than Complexes 1 and 2. For fundamental understanding, a catalytic HER mechanism is also proposed.Graphical abstract

The synthesis and characterization of tetrakis[4(4-acetlyphenoxy)phthalocyanato] cobalt (II) (1) are presented. Complex 1 together with the reported tetrakis dimethyl 5-(phenoxy)-isophthalatephthalocyaninato] cobalt (II) (2) are conjugated to carbon-based nanomaterials: graphene quantum dots (GQDs) and single-walled carbon nanotubes (SWCNTs) via π-π stacking, taking advantage of the π electrons on the graphitic structure of the nanomaterial as well as on the aromatic rings of the Co phthalocyanines (CoPcs). The electrocatalytic behaviour of the CoPcs, GQDs, SWCNTs and their respective conjugates towards the electrochemical oxidation of catechol was studied. The electrocatalytic probes were drop-dried onto the electrode surface of the glassy carbon electrode (GCE). The electrochemical oxidation of catechol was studied using cyclic voltammetry, electrochemical impedance spectroscopy and chronoamperometry. Complex 2 when linked to GQDs gave the lowest oxidation peak potentials of 0.33 V. Low catechol detection limits (LOD) of 0.057 µM was obtained for complex 2 with SWCNT. Thus, complex 2 containing more oxygen atoms outperformed complex 1 with less oxygen atoms. The CoPcs on their own showed moderate electrocatalytic behaviour, hence showing the importance of conjugating them to the carbon nanomaterials. SWCNT-based electrodes performed better than GQDs, and an improvement in the LoDs, sensitivity and the catalytic rate was observed upon conjugation.

The economic viability of the electrochemical chlorate process depends on toxic chromate to induce cathodic selectivity to hydrogen and mitigate reduction of hypochlorite or chlorate. In this study, it is shown that performance of a pilot plant for chlorate production can be sustained when a 1000-fold reduction in chromate concentration is compensated by addition of molybdate. Laboratory measurements employing a Quartz Crystal Microbalance suggest growth of a nanometre-thick hybrid Mo–Cr-oxide film to induce cathodic selectivity. An optimized energy efficiency for pilot plant operation was obtained using 0.8 mM molybdate and 27 μM chromate, balancing formation of an effective oxide layer and undesired Mo-induced decomposition of hypochlorite to oxygen in solution. Refinement at the pilot scale level is expected to further optimize the energy consumption, thereby increasing safety aspects and the economic viability of chlorate production.Graphical