Near field imaging in microwave regime using double layer split-ring resonator based metamaterial

A planar metamaterial structure consisting of two layers of split-ring resonator (SRR) arrays is demonstrated to form the image of a point source with subwavelength resolution. The source frequency is swept through the resonance gap of the metamaterial layers and the lateral field intensity distribution is recorded on the transmission side of the metamaterial. When the source is tuned to the resonance frequency of SRRs, the metamaterial acts as a high permeability medium and a distinct image with subwavelength resolution in the lateral direction is obtained. Increasing the distance between the individual SRR layers reduces the interlayer coupling, and the intensity and spatial resolution of the image decrease rapidly.     

Equilibria of formation and dehydration of the carbinolamine intermediate in the reaction of benzaldehyde with hydrazine

Measurement of polarographic limiting currents at equilibria made it possible at pH 3-7 to simultaneously determine concentrations of benzaldehyde, of its hydrazone and of the carbinolamine derivative. The dependence of concentration of carbinolamine at equilibrium on pH indicated presence of its di-, mono-, and unprotonated forms. Acid dissociation constants of the formation (pK_a¹≈3.2) of the diprotonated form and of the dissociation of the monoprotonated form of carbinolamine (pK_a²≈4.7) were estimated. The equilibrium constants of formation (K₁) and dehydration (K₂) of the carbinolamine intermediate were determined.     

Preconcentration and speciation of chromium using a melamine based polymeric sequestering succinic acid resin: its application for Cr(VI) and Cr(III) determination in wastewater

A new melamine based polymeric sequestering resin was prepared for preconcentration and separation of hexavalent chromium from water, and its sequestering action was investigated. The water-insoluble, cross-linked sequestering resin was formed by reaction with bromosuccinic acid and cross-linking of melamine. The active sequestering group on the resin is NH-(Succinic acid) or salt thereof. The resulting chelating resin was characterized by infrared spectra. The newly prepared resin quantitatively retained Cr(VI) at pH 2.0-4.0 when the flow rate was maintained between 1 and 5 ml min⁻¹. The retained Cr(VI) was instantaneously eluted with 25 ml of 0.1 M NaOH. The chromium species were determined by a flame atomic absorption spectrometer. The limits of detection for Cr(VI) and Cr(III) were found to be 5.3 and 4.2 μg l⁻¹, respectively. The precision and accuracy of the proposed procedure was checked by the use synthetic and reference steel samples. The established preconcentration method was successfully applied to the determination and selective separation of Cr(VI) in electroplating industry wastewater. Total concentrations determined by the spectrophotometric method (110.3±0.6 g l⁻¹ Cr(VI) and 1.2±0.3 g l⁻¹ Cr(III)) are compared with those found by FAAS and the obtained results (110.4±1.8 g l⁻¹ Cr(VI) and 1.4±0.5 g l⁻¹ Cr(III)) show good agreement.     

LC-ESI-MS/MS profiling of alkaloids and antiproliferative activity of Pachypoduim lamerei drake leaves

Abstract

In the present study, evaluation of the antiproliferative activity of Pachypodium lamerei Drake leaves (family Apocyaceae) against human breast cancer cell lines MDA-MB-231 was done for the total methanolic extract, crude alkaloidal mixture and ursolic acid using the MTT colorimetric assay. The methanolic extract showed the strongest antiproliferative activity followed by ursolic acid and crude alkaloidal fraction with an IC₅₀ equal to 6.2, 14.55 and 56.3?µg/ml respectively compared to oleocanthal. It is the first record for the LC/ESI-MS/MS alkaloidal profiling of the leaves of P. lamerei. Seven alkaloids were tentatively identified according to their fragmentation patterns. Four alkaloids were related to the parent indole class and two alkaloids belong to the quinoline class in addition to one steroidal alkaloid with a pregnan nucleus. Phytochemical investigation of the methanolic extract led to the isolation of three triterpenoidal compounds including ursolic acid, 11,12-didehydroursolic acid lactone and ursolic acid lactone.     

Hydrogen bonding and dimeric self-association of 2-pyrrolidinone: An ab initio study

Ab initio calculations on the different associated structures of 2-pyrrolidinone with water and with itself were carried out using 3-21G and 6-31G^* basis sets at the Hartree–Fock level, including electron correlation using second-order Møller–Plesset perturbation theory. The calculated free energy changes for the intermolecular hydrogen bonded dimer and hydrated species indicated that the molecular systems with cyclic dimerization and association with two water molecules are dominant. The results are compared to the available experimental data in the literature.     

Speciation analysis of chromium by separation on a 5-palmitoyl oxine-functionalized XAD-2 resin and spectrophotometric determination with diphenylcarbazide

The method developed in this work for the separation and preconcentration of Cr(III) is based on its retention by an Amberlite XAD-2 copolymer resin functionalized with 5-palmitoyl-8-hydroxyquinoline (oxine), abbreviated XAD-POx, with the ligand covalently bound to the copolymer. Cr(III) sorption was quantitative within the pH range 4.5–7.0 and Cr(VI) was not retained. The Cr(III) held by the resin column was eluted with a hot solution of H₂O₂ in pH9.0 aqueous NH₃–NH₄Cl buffer, and Cr oxidized to CrO₄^2– was rejected by the chelating cation-exchanger column. Any Cr(VI) originally present with Cr(III) could be reduced with an acidic solution of H₂O₂, and retained by the column yielding total Cr results, Cr(VI) being determined from the difference. The resin showed a maximal preconcentration factor of 60 for Cr(III), the LOD and LOQ being 9.3 and 30.1 nmol L^–1, respectively. The developed preconcentration-speciation analysis was finished with a diphenylcarbazide (DPC) spectrophotometric procedure suitable for conventional laboratories. The resin showed excellent salt tolerance, enabling Cr analysis in seawater, and was stable over extended use. All the interferents of this procedure that normally occur in an electroplating effluent, a blended coal CRM, and a standard steel sample could be removed by the recommended procedure, by use of partial and total selectivity at the adsorption and desorption stages, respectively, enabling preconcentration and colorimetric determination of chromium in various complex matrices.     

Investigation of Raman,FT-IR,EPR spectra and antimicrobial activity of 2-(5-H/Me/Cl-1<Emphasis Type="BoldItalic">H</Emphasis>-benzimidazol-2-yl)-phenol ligands and their Fe(NO<Subscript>3</Subscript>)<Subscript>3</Subscript> complexes

2-(5-H/Me/Cl-1H-benzimidazol-2-yl)-phenol ligands form 1:1 electrolytes, 5-coordinate monometallic complexes with iron(III) nitrate. The geometry of the [Fe(L)(OH)(H₂O)₂](NO₃) complexes was derived from theoretical calculation in DGauss/DFT level (DZVP basis set) on CACHE. In all of the complexes the ligands are bidentate, via one imine nitrogen atom and phenolate oxygen atom. The coordination is completed with a hydroxide ion, and two water molecules, adopting a distorted square pyramidal geometry. The structures of the compounds were confirmed on the basis of elemental analysis, molar conductivity, magnetic moment, FT-Raman, FT-IR (mid-IR, far-IR), EPR and u.v.–vis. The antimicrobial activities of the free ligands, their hydrochloride salts, and the complexes were evaluated using the disk diffusion method in dimethyl sulfoxide (DMSO) as well as the minimal inhibitory concentration (MIC) dilution method, against nine bacteria and the results are compared with several known antibiotic agents. Antifungal activities were reported for Candida albicans, Kluyveromyces fragilis, Rhodotorula rubra, Debaryomyces hansenii, Hanseniaspora guilliermondii, and the results were referenced against nystatin, ketaconazole, and clotrimazole antifungal agents. In most cases, the compounds tested showed broad-spectrum (Gram⁺ & Gram⁻ bacteria) activities that were either more active or as potent as the references.     

Plasma Induced Graft Polymerization of Three Hydrophilic Monomers on Nylon 6,6 Fabrics for Enhancing Antistatic Property

In this study, three hydrophilic monomers; 2-acrylamido-2-methyl-1-propanesulfonic acid, 2-hydroxyethyl methacrylate, diallyldimethylammonium chloride (DADMAC) were selected and their performance as an antistatic finish on nylon 6,6 fabrics was investigated. A non-thermal, high density atmospheric pressure plasma was used to graft polymerize the monomers on nylon 6,6 fabrics. Fabrics were first treated with solutions of monomer in water, air dried and then treated with helium plasma to graft polymerize the monomer on the fiber surface. Surface resistivity values were measured before and after soxhlet extraction with water. Results showed that the DADMAC monomer provided better antistatic properties to fabrics. Further studies with DADMAC monomer were made; effects of plasma post exposure time, plasma pre-exposure time, plasma power, concentration of the monomer and existence of a crosslinker were investigated. Higher plasma power, higher concentration of the monomer and longer post exposure times all gave better antistatic properties to the nylon 6,6 fabrics. Acid dye staining, UV–Vis and FT-IR measurements were conducted and results confirmed a grafted poly-DADMAC layer on the fabric surface.     

Oxygen bridged Homobinuclear Mn(II) compounds with Anthranilic acid: Theoretical calculations,oxidation and catalase activity

Two new homobinuclear manganese compounds with mixed ligands, [Mn₂(μ_1,1–2‐NH₂C₆H₄COO)₂(phen)₄](ClO₄)2(CH₃OH) ( 1 ), and [Mn₂(μ_1,3–2‐NH₂C₆H₄COO)₂(bipy)₄](ClO₄)2 ( 2 ) (NH₂C₆H₄COOH = anthranilic acid, bipy = 2,2′‐bipyridine, phen = 1,10‐ phenanthroline) were synthesized and thoroughly characterized by elemental analysis, IR, UV and single crystal X‐ray crystallography. X‐ray structure analysis shows that in the mono‐ and bidentate carboxylate bridged compounds, Mn–Mn distances of 1 and 2 are 3,461 Å, and 4,639 Å, respectively. The energy of the compounds was determined with a DFT (Density Functional Theory) calculation on B3LYP/6‐31G(d,p) optimized geometry by using the B3LYP/6‐31G(d,p) basis set. These compounds acts as biomimetic catalyst and show catalase‐like activity for the hydrogen peroxide dismutation at room temperature in different solvents with remarkable activity (TOF, Turnover frequency = mol of subst./(mol of cat. × time)) up to 12640 h^?1 with 1 , and 17910 h^?1 with 2 in Tris–HCl buffer). Moreover, the catalytic activity of 1 and 2 has been studied for oxidation of alcohols (cinnamyl alcohol, benzyl alcohol, cyclohexanol, 1‐octanol and 1‐heptanol) and alkenes (cyclohexene, styrene, ethyl benzene, 1‐octene and 1‐hexene) in a homogeneous catalytic system consisting t‐butylhydroperoxide (TBHP) as an oxidant in acetonitrile. Both compounds exhibited very high activity in the oxidation of cyclohexene to cyclohexanone (~80% selectivity, ~99% conversion in 1 h, TOF = 243 h^?1 and 226 h^?1) and cinnamyl alcohol to cinnamaldehyde (~64% selectivity) as the main product with very high TOF value (9180 h^?1 and 13040 h^?1 in the first minute of reaction) (~100% conversion in 0.5 h) with TBHP at 70 °C in acetonitrile, for 1 and 2 , respectively.