Cyclic voltammograms of iron and C-steels in oxalic acid solutions and investigation of the effect of phenyl phthalimide as corrosion inhibitors

Summary The electrochemical behaviour of Fe and C-steel samples in oxalic acid solutions was studied by the use of cyclic voltammetry. Two peaks were observed; the first one was the anodic peak and the second one an unexpected reductive dissolution peak which could be observed in the cathodic branch of cyclic voltammograms of all electrodes studied. The carbon content was found to increase the active dissolution of steels and to decrease their tendency towards passivation. The inhibitive efficiency of phenyl phthalimide derivatives on the active dissolution of Fe and steel samples in 0.1M oxalic acid were investigated.

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Cyclische Voltammogramme von Eisen und C-Stählen in Oxalsäurelösungen und der Einfluß von Phenylphthalimiden als Korrosionsinhibitoren

Zusammenfassung Das elektrochemische Verhalten von Eisen und C-Stählen in Oxalsäurelösungen wurde mit Hilfe cyclischer Voltammetrie studiert. Dabei treten zwei Signale auf: das anodische Signal sowie ein unerwartetes reduktives Lösungssignal. Letzteres wurde im kathodischen Zweig der cyclischen Voltammogramme aller untersuchten Elektroden gefunden. Der Kohlenstoffgehalt erhöht die aktive Auflösung von Stählen und erniedrigt ihre Tendenz zur Passivierung. Die Inhibitionseffizienz von Phenylphthalimiden für die aktive Auflösung von Eisen und Stahlproben in 0.1M Oxalsäure wurde untersucht.

     

Deposition of ZnS thin film by ultrasonic spray pyrolysis: effect of thickness on the crystallographic and electrical properties

Zinc sulfide (ZnS) thin films have been deposited on Si (1 0 0) substrate using ultrasonic spray pyrolysis. X-ray diffraction (XRD) analysis revealed that the films are (0 0 2) preferentially oriented with c-axis-oriented wurtzite structure. The crystallinity has been found to improve with film thickness in the 180–6000 nm range. Film structure has been analyzed by XRD, scanning electron microscope, FTIR, and Raman spectroscopies, while the stoichiometry has been verified by energy-dispersive spectroscopy and particle-induced X-ray emission techniques. Electrical properties of the grown films were characterized by current–voltage and capacitance–voltage measurements where, the films show better conducting behavior at higher thickness.     

Development of new high‐performance visible light photoinitiators based on carbazole scaffold and their applications in 3d printing and photocomposite synthesis

In this article, new compounds based on the carbazole scaffold (DMs = DM1 and DM2, constituted by a carbazole unit connected on positions 3 and 6 to a two 4,4′‐dimethoxydiphenylamine groups and differing by the substituent present on the nitrogen heteroatom of the carbazole core) were synthesized and proposed as high‐performance visible light photoinitiators/photosensitizers for both the free‐radical polymerization of methacrylates and the cationic polymerization of epoxides upon visible light exposure using LED@405 nm. Remarkably, DM2 leads to higher final conversions than DM1. In order to study the photophysical and photochemical properties of the carbazole derivatives, different parameters were taken into account such as the light absorption, the steady‐state photolysis, and the fluorescence spectroscopy. Using different techniques such as fluorescence quenching, redox behavior, and cyclic voltammetry, we are able to discuss the photosensitization/photoinitiation reactions providing a full coherent picture of the involved chemical mechanisms. The photosensitization of the carbazole derivatives occurred predominantly via singlet excited states at the rate of the diffusion limit. Upon exposure to laser diode at 405 nm, DMs show high performance in initiating systems for 3D resins. Remarkably, DM2 can also be used in photocomposite synthesis using light‐emitting diode conveyor. © 2019 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2019, 57, 2081–2092     

Buprofezin dissipation and safety assessment in open field cabbage and cauliflower using GC/ITMS employing an analyte protectant

An analytical method for the determination of buprofezin residues in cabbage and cauliflower was developed and validated using gas chromatography with ion trap mass spectrometry. The analyte protectant d ‐sorbitol was used at a concentration level of 0.5 mg mL^?1 in acetonitrile instead of in matrix for constructing the calibration curves of the buprofezin standard. The average recoveries ranged from 91.3 to 96.8%, with an RSD of ≤2.7%. The limits of detection and quantitation of the method in cabbage and cauliflower were 1.3, 1.7 and 4.3, 6.2 μg kg^?1, respectively. The residual levels and dissipation kinetics of buprofezin 25% wettabe powder in cabbage and cauliflower cultivated under open field conditions was investigated at the single (T1) and double (T2) recommended rates of application. Half‐life periods were found to be 1.73 and 2.1 days in cabbage, whereas in cauliflower, these values were 1.85 and 2.36 days at T1 and T2, respectively. Based on the dissipation study, and the maximum residue limit value of 0.05 mg kg^?1, the proposed pre‐harvest interval of buprofezin in cabbage was 3–6 days and that in cauliflower was 4–10 days. The results showed that buprofezin is safe for application at both recommended application rates.     

Solid–liquid phase equilibria for binary mixtures of propellant’s stabilizers

Solid–liquid equilibria for three binary mixtures of N-(2-acetoxyethyl)-p-nitroaniline (1) + 2-nitrodiphenylamine (2), N-(2-acetoxyethyl)-p-nitroaniline (1) + ethyl centralite (2) and N-(2-acetoxyethyl)-p-nitroaniline (1) + methyl centralite (2) have been determined experimentally using differential scanning calorimeter (DSC). Simple eutectic behaviours for these systems have been observed. The experimental results have been correlated by means of NRTL and UNIQUAC equations. The root-mean-square deviations of the solubility temperatures for all measured data vary from 0.61 to 3.32 K and depend on the particular model used. The best solubility correlation has been obtained with the UNIQUAC model.     

In vitro surface biocompatibility of high-content silicon-substituted calcium phosphate ceramics

The present work investigates surface biocompatibility of silicon-substituted calcium phosphate ceramics. Different silicon-substituted calcium phosphate ceramic bodies were prepared from co-precipitated powders by sintering at 1300°C. The in vitro bioactivity of the ceramics was assessed in simulated body fluid (SBF) at 37°C for periods up to 4 weeks. The changes in the surface morphology and composition were determined by scanning electron microscopy (SEM) coupled with electron probe microanalysis and energy dispersive spectrometer (EDX). Inductively coupled plasma optical emission spectroscopy (ICP-OES) was used to observe the change in ionic concentration of SBF after removal of the samples. The bioactivity of the ceramics increased with an increasing silicate ion substitution in a systematic way. The surface of ceramics with 2.23% silicon substitution was partially covered with apatite layer after one week, while ceramics with 8.1% silicon substitution were completely covered with apatite in the first week. The porous microstructure of high-concentration Si-substituted ceramics helps the dissolution of surface ions and the leaching process. This allows SBF to reach supersaturation in a short time and accelerate the deposition of apatite layer.      

5‐O‐Caffeoylshikimic acid from Solanum somalense leaves: Advantage of centrifugal partition chromatography over conventional column chromatography

Solanum somalense leaves, used in Djibouti for their medicinal properties, were extracted by MeOH. Because of the high polyphenol and flavonoid contents of the extract, respectively, determined at 80.80 ± 2.13 mg gallic acid equivalent/g dry weight and 24.4 ± 1.01 mg quercetin equivalent/g dry weight, the isolation and purification of the main polyphenols were carried out by silica gel column chromatography and centrifugal partition chromatography. Column chromatography led to 11 enriched fractions requiring further purification, while centrifugal partition chromatography allowed the easy recovery of the main compound of the extract. In a solvent system composed of CHCl₃/MeOH/H₂O (9.5:10:5), 21.8 mg of this compound at 97% purity was obtained leading to a yield of 2.63%. Its structure was established as 5‐O‐caffeoylshikimic acid by mass spectrometry and NMR spectroscopy. This work shows that S. somalense leaves contain very high level of 5‐O‐caffeoylshikimic acid (0.74% dry weight), making it a potential source of production of this secondary metabolite that is not commonly found in nature but could be partly responsible of the medicinal properties of S. somalense leaves.     

Facile synthesis of silver doped-copper oxide nano materials utilizing areca catechu (AC) leaf extract and their antidiabetic and anticancer studies

The present research highlights physical significance of green combination of metal oxide nanomaterials utilizing medicinal plant which has widely analyzed in different medical applications i.e., medicinal science, therapeutics. In this paper, we discussed environmentally benign approach for synthesizing silver doped copper oxide nanoparticles (Ag–CuO NPs) utilizing (ACLE). Scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM) and energy dispersive spectroscopy (EDS) were utilized to confirm the size, crystalline structure and surface morphology of the obtained nanomaterials. The monoclinic crystalline structure of the Ag–CuO NPs as produced was revealed by XRD patterns. Morphological analysis disclosed the nano-based spherical configuration of Ag–CuO NPs, as well as their morphology and elemental composition. The anti-diabetic effect of Ag–CuO NPs was further investigated utilizing a yeast cell model and amylase inhibition. Here, a decrease in intracellular glucose and a delay in carbohydrate digestion indicate promising antidiabetic action. Furthermore, the prepared nanomaterial showed anticancer potential against the MCF-7 cancer cell line, with an IC ₅₀ value of 11.21 g/ml.     

Novel Potentiometric Solid-contact Electrode for the Determination of Fe2+ Ions via MWCNTs-Gemifloxacin Composite

A novel electrode was fabricated for the quantitation of Fe²⁺ ion. It was based on the covalent attachment of the gemifloxacin molecule (the recognition element) to the surface of MWCNTs to be incorporated as an electroactive material. Linear response of Fe²⁺ ions was found in the concentration range of 1×10⁻² mol L⁻¹ to 1×10⁻⁸ mol L⁻¹ with a Nernstian slope of 30.37 ±0.3 (mV/decade) and attained a stable response within 5 s. The sensor exhibited LOD value of 4.8×10⁻⁹ mol L⁻¹. It was applied in the monitoring of Fe²⁺ concentration in multi-vitamins tablets, tap water and milk samples with acceptable recovery ranged from 94.00 % to 102.00 %.