Enzymes and phytochemicals from neem extract robustly tuned the photocatalytic activity of ZnO for the degradation of malachite green (MG) in aqueous media

The malachite green (MG) is very difficult to degrade in water; thus, it needs an efficient photocatalyst. In this study, neem extract was used to tune the surface and crystal properties of ZnO nanostructures for the photodegradation of MG. The biosynthesized ZnO samples were prepared by hydrothermal method in the presence of 5, 10 and 15 mL of neem extract. The structural characterization has shown nanoparticle like morphology of ZnO as revealed by scanning electron microscopy (SEM) and hexagonal phase was confirmed by powder X-ray diffraction (XRD) technique. The XRD analysis has shown a shift in the 2 theta towards lower angle for ZnO with increasing amount of neem extract. Also, the crystallite particle size of ZnO was decreased with increasing neem extract. The UV–visible spectroscopy has shown the decrease in the optical band gap of ZnO, and the lowest band gap is possessed by ZnO sample produced with 15 mL of neem extract. The ZnO sample obtained with 15 mL of neem extract has shown approximately 99% degradation efficiency for MG for 70 min in aqueous solution. The superior photocatalytic activity of ZnO sample with 15 mL of neem extract could be attributed from the decrease in charge recombination rate due to the decreased optical band gap and particle size.

     

Nd(III) and Gd(III) Sorption on Mesoporous Amine-Functionalized Polymer/SiO2 Composite

The strong demand for rare-earth elements (REEs) is driven by their wide use in high-tech devices. New processes have to be developed for valorizing low-grade ores or alternative metal sources (such as wastes and spent materials). The present work contributed to the development of new sorbents for the recovery of rare earth ions from aqueous solutions. Functionalized mesoporous silica composite was synthesized by grafting diethylenetriamine onto composite support. The physical and chemical properties of the new sorbent are characterized using BET, TGA, elemental analysis, titration, FTIR, and XPS spectroscopies to identify the reactive groups (amine groups: 3.25 mmol N g⁻¹ and 3.41 by EA and titration, respectively) and their mode of interaction with Nd(III) and Gd(III). The sorption capacity at the optimum pH (i.e., 4) reaches 0.9 mmol Nd g⁻¹ and 1 mmol Gd g⁻¹. Uptake kinetics are modeled by the pseudo-first-order rate equation (equilibrium time: 30–40 min). At pH close to 4–5, the sorbent shows high selectivity for rare-earth elements against alkali-earth elements. This selectivity is confirmed by the efficient recovery of REEs from acidic leachates of gibbsite ore. After elution (using 0.5 M HCl solutions), selective precipitation (using oxalate solutions), and calcination, pure rare earth oxides were obtained. The sorbent shows promising perspective due to its high and fast sorption properties for REEs, good recycling, and high selectivity.     

Photosensitized generation of singlet oxygen from rhenium(I) and iridium(III) complexes

Photophysical properties in dilute acetonitrile solution are reported for a number of iridium(III) and rhenium(I) complexes. The nature of the lowest excited state of the complexes under investigation is either metal-to-ligand charge transfer ((3)MLCT) or a ligand centred ((3)LC) state. Rate constants, k(q), for quenching of the lowest excited states by molecular oxygen are in the range 1.5 x 10(8) to 1.4 x 10(10) M(-1) s(-1). Efficiency of singlet oxygen production, f(Delta)(T), following oxygen quenching of the lowest excited states of these complexes, are in the range of 0.27-1.00. The rate constants and the efficiency of singlet oxygen formation are quantitatively reproduced by a model that assumes the competition between a non-charge transfer (nCT) and a CT deactivation channel. The balance between CT and nCT deactivation channels, which is described by the relative contribution p(CT) of CT induced deactivation, is discussed. The kinetic model is found to be successfully applied in the case of quenching of the excited triplet states of coordination compounds by oxygen in acetonitrile, as was proposed for the quenching of pi-pi* triplet states by oxygen.     

Spectrophotometric determination of gatifloxacin in pure form and in pharmaceutical formulation

Simple, rapid, and extractive spectrophotometric methods were developed for the determination of gatifloxacin (GT) in bulk and pharmaceutical dosage form. These methods are based on the formation of yellow ion-pair complexes between the basic nitrogen of the drug and three sulphonphthalein acid dyes, namely; bromocresol green (BCG), bromocresol purple (BCP), bromophenol blue (BPB) and bromothymol blue (BTB) in phthalate buffer pH 3.0, 3.4 and 3.2, using BCG, BCP and (BPB or BTB), respectively. The formed complexes were extracted with chloroform and measured at 415, 417, 412 and 414 nm for BCG, BPB, BCP and BTB, respectively. The analytical parameters and their effects on the reported systems are investigated. The reactions were extremely rapid at room temperature and the absorbance values remains unchanged at 48 h for all reactions. Beer's law was obeyed in the ranges 2.0-20, 2.0-14 and 2.0-16 microg mL(-1) for BCG, BCP and (BPB or BTB), respectively. The composition of the ion pairs was found 1:1 by Job's method. Beer's law validation, accuracy, precision, limits of detection, limits of quantification. The proposed methods have been applied successfully for the analysis of the drug bulk form and its dosage form. The results were in good agreement with those obtained by the official and reported methods.     

Electrocatalytic Nitrite Determination Using Iron Phthalocyanine Modified Gold Nanoparticles

Electrochemical detection of nitrite was achieved via electrodeposition of gold nanoparticles (AuNPs) onto glassy carbon electrodes, followed by 3‐mercaptopropionic acid (MPA) self‐assembly, enabling attachment of an iron(III) monoamino‐phthalocyanine (FeMAPc) catalyst via amide bond formation. The use of scanning electron microscopy, energy dispersive X‐ray spectroscopy and ultraviolet‐visible spectroscopy realised surface characterisation while cyclic voltammetry and electrochemical impedance spectroscopy techniques were applied for electrochemical interrogation. The electrochemical behaviour of nitrite at the bare (GCE), AuNPs/GCE, FeMAPc/GCE and FeMAPc‐MPA/AuNPs/GCE was further scrutinised using differential pulse voltammetry in phosphate buffer solution (0.1 M PBS, pH 5.8). Overall the FeMAPc‐MPA/AuNPs/GCE resulted in sensitivity 14.5 nA/µM, which was double that of AuNPs/GCE, 2.4 times FeMAPc/GCE and 3.5 times the response at a bare GCE, with linear range 1.9 µM–2.04 mM (PBS, pH 5.8) and LOD 0.21 µM. An interference study revealed that the proposed sensor (FeMAPc‐MPA/AuNPs/GCE) exhibited a selective response in the presence of interfering anions and the analytical capability of the sensor was demonstrated via nitrite ion determination in real water samples.     

High-performance thin-layer chromatographic determination of trigonelline content in various extracts and different varieties of some commercial coffees available in the Saudi Arabian market

JPC – Journal of Planar Chromatography – Modern TLC - The proposed research study was undertaken to establish a simple, rapid and sensitive high-performance thin-layer chromatography...     

Selective cyclization of S-substituted pyrimidinethione: Synthesis and antimicrobial evaluation of novel polysubstituted thiazolopyrimidine and thiazolodipyrimidine derivatives

The synthetic strategy is based on alkylation of 4-aryl-N-(4-chlorophenyl)-6-methyl-2-thioxo-1,2,3,4-tetrahydropyrimidine-5-carboxamide derivatives IV a–g , with some alkyl halides and α-haloketones, namely, methyl iodide, chloroacetonitrile, and phenacyl bromide to give the corresponding S-substituted derivatives Va–c . Treatment of IVa–c with ethyl bromoacetate in ethanol under reflux in the presence of potassium hydroxide solution led to the formation of N-(4-chlorophenyl)-7-methyl-3-oxo-5-(aryl)-2,3-dihydro-5H-thiazolo[3,2-a]pyrimidine-6-carboxamide derivative VIII a–c in a single-step synthesis. On the other hand, compound IVa reacted with α-halo carbonitriles, namely, chloro acetonitrile, and monobromo malononitrile, to produce directly thiazolo[3,2-a]pyrimidine derivatives Xa and Xb , respectively, Compound Xb also reacted with each of formic acid, formamide, and ammonium thiocyanate to form thiazolodipyrimidine derivatives XI–XIII , respectively. Compound VIIIa–c coupled with arenediazonium salts in pyridine to give the corresponding 2-arylhydrazo derivatives XVIa–e . Compounds IV a–g and VIIIa–c were resynthesized under microwave irradiation. Some of the newly synthesized compounds were tested for their antimicrobial activities.     

Copper vanadate nanowires-based MIS capacitors: synthesis,characterization, and their electrical charge storage applications

Dielectric properties of porous glass nanocomposites with TGS crystals embedded into six porous matrices with average pore size from 5 to 312 nm were investigated in the temperature range from 280 to 380 K at selected frequencies. The results are discussed based on the effect of the particle size on the phase transition temperature of TGS nanocomposites. Temperature–size phase diagram of TGS composites was derived. Non-monotonic character of the temperature-driven phase transition (T _p) with the decreasing particle size was determined. The nature of the T _p variation can be ascribed to the size-effect theoretically predicted by Zhong et al. (Phys Rev B 50:698–703, 1994).     

The ground state energy of the three-dimensional Ginzburg-Landau model in the mixed phase

We consider the Ginzburg-Landau functional defined over a bounded and smooth three-dimensional domain. Supposing that the strength of the applied magnetic field varies between the first and second critical fields, in such a way that HC₁?H?HC₂, we estimate the ground state energy to leading order as the Ginzburg-Landau parameter tends to infinity.