Volume 23 (2021): Issue 1 (March 2021)

Sepiolite and the sepiolite-based materials were studied in terms of carbon dioxide adsorption. The pore structure and the surface characterization of the obtained materials were specified based on adsorption-desorption isotherms of nitrogen measured at –196^oC and carbon dioxide at 0^oC. The specific surface area (SSA) was calculated according to the BET equation. The pore volume was estimated using the DFT method. Pristine sepiolite has shown the following value of SSA and CO₂ uptake at 0oC – 105 m²/g and 0.27 mmol/g, respectively. The highest value of these parameters was found for material obtained by KOH activation of mixture sepiolite and molasses (MSEP2) – 676 m²/g and 1.49 mmol/g. Sample MSEP2 also indicated the highest value of total pore volume and micropores volume with a diameter up to 0.8 nm.

Four new symmetrical Schiff bases derived from 2,2’-diamino-4,4’-dimethyl-1,1’-biphenyl-salicylaldehyde have been synthesized and characterized by elemental analysis and different spectroscopic techniques. The reaction of 2,2’-diamino-4,4’-dimethyl-1,1’-biphenyl with two equivalents of 5-tert-butyl-, 3,5-dinitro-, 3,5-dibromo- and 3-tert-butyl-salicylaldehyde yielded 2,2’-bis(5-tert-butyl-salicylideneamino)-4,4’-dimethyl-1,1’-biphenyl (A1) as well as the 3,5-dinitro- (A2), 3,5-dibromo- (A3) and 3-tert-butyl- (A4) substituted derivatives. The tetradentate ligands were then reacted with copper-, manganese- and zinc-acetate producing the tetra-coordinate metal complexes which were characterized by FTIR, UV-Visible spectroscopy, magnetic susceptibility and elemental analysis. Zinc complexes were characterized by 1H-NMR spectroscopy. Density functional theory (DFT) calculations at the B3LYP/6-31G(d) level of theory were carried out to fully optimize and examine the molecular geometries of complexes. Subsequently, IR vibrational and UV-Vis absorption spectra were computed and correlated with the observed values and the results are in good agreement with the experimental data. The anticancerous and antiproliferative activity of the A3 ligand and its metal complexes were determined.

The research study investigated the biosorption behavior of Pb(II) ions by treated and untreated biomass of B. subtilis. At initial biosorption conditions, the biosorption efficiency was found to be 36.75%. At the optimized experimental conditions, control biomass showed maximum biosorption efficiency of 58.04% where the biomass was treated with different chemicals. The biomass treated with formaldehyde showed the highest efficiency of 80.9% which was further optimized and attained maximum efficiency of 89.8% for Pb(II) ions. SEM (Scanning Electron Microscope) and EDX (Energy dispersive X- ray) analysis evaluates the structural and elemental changes that occurred as a result of biosorption. Functional groups that are involved in biosorption were revealed by FTIR (Fourier Transform Infrared spectroscopy). Kinetic data showed the best fit with the pseudo second-order model. Effective removal of lead ions from industrial contaminated water sources by pretreatment biomass of B. subtilis elucidates its potential use as biosorbent for metal remediation..

Plant-esterase (EC 3.1.1.X) has received much attention because plant esterase and acetylcholinesterase (AChE) share a similar sensitivity towards organophosphorus (OP) pesticides detection with the same inhibition mechanism. To improve the analytical performance, tetraphenyl metal porphyrin, as an indicator was introduced to combine with plant-esterase. The time of reach equilibrium in PBS solution was shortened after adding plant-esterase by assaying the intensify change of the porphyrin spectrum. Meanwhile, intensify of porphyrin spectrum with plant-esterase was increased compared with that of only the porphyrin spectrum in solution. Tetraphenyl metal porphyrin, such as cobalt(II) meso-tetraphenyl porphyrin, is a mixed reversible inhibitor of plant-esterase from kinetic parameters. The combination ratio of plant-esterase and porphyrin is 2:1. On the other hand, the interaction between CoTPPCl and plant-esterase is the strongest among all tested tetraphenyl metal porphyrin. And the mixed system (CoTPPCl-plant-esterase) showed the best sensitivity towards the tested pesticide. All these results indicated that a complex system composed of tetraphenyl metal porphyrin and plant-esterase was fit for detecting pesticides. They make meaningful guidance on the further design of sensing material in monitoring pesticides.

Very fast reactions of forming higher nitrogen oxides set out an equilibrium framework for the course of the reaction of nitrogen monoxide oxidation. The slow course of reaction of nitrogen monoxide with oxygen permanently violates the created equilibria. In particular, the equilibrium of the oxidation reaction of nitrogen monoxide with nitrogen dioxide. The contribution of this reaction to the transformation of nitrogen monoxide in the conditions of nitrogen trioxide removal from the gas phase was estimated.

Spent Pot Lining (SPL) cathode pot, waste from the aluminium smelting process needs detoxification from cyanides, washing out water-soluble salts and extraction of the cryolite (Na₃AlF₆) decomposition products to be recycled. Revealed cryolite decomposition mechanism with NaOH opens possibilities to explore its critical role in the reactive extraction process. Common Na⁺ ion from NaOH hinders the solubility of the product but also drives mass transfer to the reaction site. Reaction mass balance provides adequate liquid to solid ratio (L/S) and NaOH concentration range. A newly developed kinetic model based on Whitman film theory and NaOH mass flow enables prediction of the reaction time to decompose cryolite to a low enough level. Results show that the internal particle resistance to transport (1/k_s) is 19 times larger than the external (1/k_l) one and governs the whole process.

New five ciprofloxacin (CIP) complexes of dioxouranium(II), oxozirconium(II), zirconium(IV), oxovanadium(II) and vanadium(IV) in the proportion 1:2 have been prepared using CIP as a drug chelate with UO₂(NO₃)₂. 6H₂O, ZrOCl₂. _8H2O, ZrCl₄, VOSO₄. xH₂O and V₂O₅ respectively. The CIP complexes have been characterized based on the elemental analysis, molar conductance, magnetic, (FTIR & ¹HNMR) spectral and thermal studies. The molar conductance studies of the synthesized complexes in DMSO solvent with concentration of 10^–3 M indicate their non-electrolytic properties. At room temperature, the magnetic moment measurements revealed a diamagnetic behavior for all CIP prepared complexes. The different formulas of the new complexes can be represented as [UO₂(CIP)₂(NO₃)₂] (I), [VO(CIP)₂(SO₄)(H₂O)] (II), [V₂(O)(O₂)₂(CIP)₂] (III), [Zr(O)(CIP)₂(Cl)₂] (IV), and [Zr(CIP)₂(Cl)₄] (V). The thermal analysis data of the complexes indicates the absence of coordinated water molecules except for vanadyl(II) complex (II). The CIP chelate is a uni-dentate ligand coordinated to the mentioned metal ion through terminal piperazinyl nitrogen. The transmission electron microscopy (TEM) investigation confirms the nano-structured form of the complexes.

Synthesis of ethyl 7-hydroxy-1-azacoumarin-3-carboxylate (3) was developed using ethyl-7-hydroxy coumarin-3-carboxylate and ammonium solution as the key synthons. Condensation of ethyl 7-hydroxy-1-azacoumarin-3-carboxylate with ammonium acetate and aniline to give N-substituted-7-hydroxy-1-azacoumarin-3-carboxamides (7-Hydroxy -1-azacoumarin-3-carboxamide (4) and N-phenyl 7-Hydroxy-1-azacoumarin-3-carboxamide (5)). Bromo derivative (N-phenyl 6, 8-dibromo-7-hydroxy-1-azacoumarin-3-carboxamide (6)) was obtained from halogenation of compound N-phenyl 7-Hydroxy-1-azacoumarin-3-carboxamide (5) with bromine in glacial acetic acid. N-phenyl-2,5-diacetoxy-6, 8-disubstituted-Quinoline-3-carboxamides (N-phenyl 2,7-diacetoxy-Quinoline-3-carboxamide (7) and N-phenyl 2,7-diacetoxy-6,8-dibromo-Quinoline-3-carboxamide (8)) were prepared via the acetylation of compounds 5 and 6 with acetic anhydride. Five compounds 4–8 were evaluated in vitro against more than one human tumor cell lines. Among the selected compounds, 6 showed the best in vitro cytotoxicity against the human cancer cell line; MCF-7 (with IC₅₀ = 10.12 μM). In addition, cell cycle analysis of compound 6 demonstrated cell cycle arrest at G2/M phase and Pre-G1 apoptosis.

Trimethoprim drug (TMP) complexes of copper (II), cobalt (II), and nickel (II) were prepared and discussed by using elemental analysis (C, H, N analysis), magnetic, molar conductance, FTIR, Raman spectroscopy, electron spin resonance (ESR) and UV-vis spectroscopy analyses. TMP drug coordinated as a tridentate ligand towards the respected three metal ions through two nitrogen atoms of amino groups and nitrogen atom of pyrimidine ring which flanked between –NH₂ groups, these assignments confirmed by spectroscopic, magnetic, ESR and thermogravimetric analyses with formulas [Cu(TMP)(H₂O)₃]Cl₂, [Co(TMP)(H₂O)₃]Cl₂ and [Ni(TMP) (H₂O)]Cl₂. Copper (II) and cobalt (II) complexes have an octahedral geometrical structure included one TMP molecule, three coordinated water molecules and two uncoordinated chlorine atoms while, nickel(II)–TMP complex has a tetrahedral geometric configuration that involved one TMP molecule, one coordinated water molecule and two uncoordinated chlorine atoms. The activation energies and other kinetic thermodynamic parameters were estimated based on the employed of the Coats-Redfern and Horowitz-Metzger equations. The nano–structured form of the synthesized TMP complexes was confirmed dependent on the transmission electron microscopy (TEM).