An Under-Appreciated Source of Reproducibility Issues in Cross-Coupling: Solid-State Decomposition of Primary Sodium Alkoxides in Air

The decomposition of primary sodium alkoxide salts under ambient storage conditions and the effects of this phenomenon on commonly employed transition-metal-catalyzed cross-coupling reactions are described. By utilizing NMR, IR, and Raman spectroscopy, along with a modified Karl Fischer analysis, the main inorganic degradants were characterized, and CO₂ in the air was found to be a critical reactant within the decomposition process. The effects of storage conditions on decomposition were evaluated, and the preliminary experiments to understand the kinetics of this process were performed.

An Under-Appreciated Source of Reproducibility Issues in Cross-Coupling: Solid-State Decomposition of Primary Sodium Alkoxides in Air

The decomposition of primary sodium alkoxide salts under ambient storage conditions and the effects of this phenomenon on commonly employed transition-metal-catalyzed cross-coupling reactions are described. By utilizing NMR, IR, and Raman spectroscopy, along with a modified Karl Fischer analysis, the main inorganic degradants were characterized, and CO₂ in the air was found to be a critical reactant within the decomposition process. The effects of storage conditions on decomposition were evaluated, and the preliminary experiments to understand the kinetics of this process were performed.

Facile Synthesis of Phase Tunable MoO3 Nanostructures and Their Electrochemical Sensing Properties

MoO3 nanostructures with tunable phases such as α-MoO3, β-MoO3 and their mixed phases were synthesized via a simple solid state decomposition method and employed as electrocatalyst for the detection of biomolecule. The phase and crystal structure of the synthesized MoO3 nanostructures were confirmed through X-ray diffraction (XRD) studies. The MoO3 nanostructures were also characterized by Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and UV-Vis spectroscopy for their structural, chemical state and optical properties, respectively. The observed results confirmed the successful formation of phase tunable MoO3 nanostructures. The surface texture and morphology of the samples was characterized by field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). The obtained images showed the formation of hexagons, cubes and rods morphology of MoO3. The synthesized MoO3 nanostructures were used to modify the surface of glassy carbon electrode (GCE) to detect biomolecule (quercetin).

An in situ study on the solid state decomposition of ammonia borane: unmitigated by-product suppression by a naturally abundant layered clay mineral

Borazine is a by-product often encountered in the thermal decomposition of ammonia borane, which leads to an inescapable hindrance towards sustainability and cost effectiveness.

Thermal degradation kinetics of poly(arylene ether nitrile) and its cross-linked polymer

The kinetics of the thermal degradation of poly(arylene ether nitrile) (PEN; cross-linked and uncross-linked) was investigated by thermogravimetric analysis. The corresponding kinetic parameters of PEN were determined using the Flynn–Wall–Ozawa and the Friedman method. The Satava method was also used to explore the probable degradation mechanisms of PEN. The results showed that the activation energy ( E) obtained from the Flynn–Wall–Ozawa method was in good agreement with the value obtained from the Friedman method. The solid-state decomposition mechanisms of uncross-linked and cross-linked PEN were A2 (nucleation and growth) and R2 type (phase boundary–controlled reaction), respectively. The E and initial decomposition temperature of cross-linked PEN were higher than those of uncross-linked PEN, which indicates that cross-linking treatment is effective in enhancing the thermal stability of PEN.