Environmentally Benign Synthesis of 2-Pyrazolines and Cyclohexenones Incorporating Naphthalene Moiety and Their Antimicrobial Evaluation

We reported the environmental benign synthesis of chalcones,2-pyrazolines and cyclohexanones under microwave irradiation.Chalcones were obtained by the condensation of each of 2-hydroxyacetophenone derivatives with a-naphthaldehyde under microwave irradiation.The condensation reactions of each of synthesized chalcones with phenyl hydrazine under microwave irradiation in the presence of dry acetic acid as a cyclizing agent gave 2-pyrazolines.Also,the new cyclohexenone derivatives,valuable intermediates to synthesize fused heterocycles,have been prepared by the cyclocondensation of each of hydroxychalcones with ethyl acetoacetate.The structures of the synthesized compounds were elucidated by infrared（IR） spectrometry,nuclear magnetic resonance（NMR）,mass spectrometry（MS） and elmental analysis.The results indicate that unlike classical heating,microwave irradiation results in higher yields with shorter and cleaner reactions.The synthesized compounds were screened for antimicrobial activity against Staphylococcus aureus,Escherichia coli,Candida Albicans and Aspergillus niger.We clarified the effects of different substituents in the tested compounds on the obtaind antibacterial activities and antifungal activities.     

Flexural,impact, rheological and physical characterizations of POM reinforced by carbon nanotubes and paraffin oil

The paraffin oil dispersion technique innovated in the recent years to synthesize bulk polymer nanocomposite materials has a uniform dispersion. This research work aims to study the effect of added carbon nanotubes (CNTs) on flexural, impact and rheology behaviors of polyoxymethylene (POM) reinforced by 0–0.03 wt% of CNT using paraffin oil dispersion technique. The wettability and lamellar thickness were measured and rheological performance investigated using a parallel plate rheometer. The flexural and impact mechanical properties were also evaluated. The fracture surfaces were then examined by microscopy. The results showed that the energy to break, flexural strength and modulus increased proportionally with the addition of the amount of CNT in the matrix. For the rheology behavior, the viscosity decreased at the low percentage of CNT and then increased with increase in the percentage weight ratio of CNT in the POM matrix. It was also noted that the water contact angle rose with the increase the CNT percentages. Copyright © 2016 John Wiley & Sons, Ltd.     

Ni(II), Co(II), and Cu(II) complexes incorporating 2-pyrazinecarboxylic acid：Synthesis,characterization, electrochemical evaluation,and catalytic activity for the synthesis of 2H-indazolo[2,1-b]phthalazine-triones

Three complexes containing 2-pyrazinecarboxylate (pzca–), including [Ni(pzca)2(H2O)2], [Co(pzca)2(H2O)2], and [Cu(pzca)2(H2O)2], have been synthesized and characterized using physico-chemical and spectroscopic methods. Furthermore, the structure of each complex was determined by single-crystal X-ray diffraction. All three complexes have an octahedral geometry, where the metal ion chelated by two carboxylate oxygens, two nitrogen atoms belonging to pyrazinic acid molecules, and two oxygen atoms of two water molecules. The catalytic activities of these complex-es were also investigated in the green synthesis of 2H-indazolo[2,1-b]phthalazine-triones by the reaction of hydrazine hydrate with an arylaldehyde, phthalic anhydride, and dimedone in acetic acid.     

Simulation of conjugate radiation–forced convection heat transfer in a porous medium using the lattice Boltzmann method

In this paper, a lattice Boltzmann method is employed to simulate the conjugate radiation–forced convection heat transfer in a porous medium. The absorbing, emitting, and scattering phenomena are fully included in the model. The effects of different parameters of a silicon carbide porous medium including porosity, pore size, conduction–radiation ratio, extinction coefficient and kinematic viscosity ratio on the temperature and velocity distributions are investigated. The convergence times of modified and regular LBMs for this problem are 15 s and 94 s, respectively, indicating a considerable reduction in the solution time through using the modified LBM. Further, the thermal plume formed behind the porous cylinder elongates as the porosity and pore size increase. This result reveals that the thermal penetration of the porous cylinder increases with increasing the porosity and pore size. Finally, the mean temperature at the channel output increases by about 22% as the extinction coefficient of fluid increases in the range of 0–0.03.

     

Structural and optoelectronic properties of amorphous GaN thin films

Amorphous gallium nitride (a-GaN) thin films were deposited on glass substrate by electron beam evaporation technique at room temperature and high vacuum using N ₂ as carrier gas. The structural properties of the films was studied by X-ray diffraction (XRD) and scanning electron microscope (SEM). It was clear from XRD spectra and SEM study that the GaN thin films were amorphous. The absorbance, transmittance and reflectance spectra of these films were measured in the wavelength range of 300–2200 nm. The absorption coefficient spectral analysis in the sharp absorption region revealed a direct band gap of E _g = 3:1 eV. The data analysis allowed the determination of the dispersive optical parameters by calculating the refractive index. The oscillator energy E ₀ and the dispersion energy E _d, which is a measure of the average strength of inter-band optical transition or the oscillator strength, were determined. Electrical conductivity of a-GaN was measured in a different range of temperatures. Then, activation energy of a-GaN thin films was calculated which equalled E _a = 0:434 eV.     

A new liquid membrane electrode for determination of vitamin B1 in multivitamin preparations

Summary A new liquid membrane electrode was developed which is highly selective and sensitive for vitamin B₁. It is based on the thiamine-picrolonate ion-pair complex as an electroactive material in nitrobenzene solvent. The electrode has a remarkable selectivity for vitamin B₁ in the presence of vitamins B₂, B₆, B₁₂ and nicotinamide. The results obtained for the determination of vitamin B₁ in various multivitamin preparations at levels as low as 1 g/ml show an average recovery of 98% (mean standard deviation 1.8%) and are favourably compared with those obtained by the official methods.

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Neue Flüssig-Membranelektrode zur Bestimmung von Vitamin B₁ in Multivitaminpräparaten

Zusammenfassung Eine neue, für Vitamin B₁ hochselektive Flüssig-Membranelektrode wurde entwickelt. Sie beruht auf dem Thiamin-Picrolonat-Ionenpaarkomplex als elektroaktives Material im Lösungsmittel Nitrobenzol. Die Elektrode besitzt eine beachtliche Selektivität für Vitamin B₁ in Gegenwart der Vitamine B₂, B₆, B₁₂ und Nicotinamid. Bei Bestimmungen in verschiedenen Multivitaminpräparaten mit Konzentrationen bis herab zu 1 g/ml erhielt man eine durchschnittliche Wiederfindung von 98% (mittlere Standardabweichung 1,8%). Die erhaltenen Resultate zeigen gute Übereinstimmung mit den nach amtlichen Methoden erhaltenen Werten.

     

Spectrophotometric determination of phosphorus and arsenic in pharmaceutical organic compounds

Summary A simple and accurate method is described for the microdeter-mination of phosphorus and arsenic in some pharmaceutical organic compounds. It is based on the conversion of phosphorus and arsenic into phosphate and arsenate ions respectively, followed by precipitation with quinoline and sodium molybdate reagents. The excess quinoline in the supernatant is spectrophotometrically measured at 312.5 nm in an ammonium acetate background of pH 5.5. The results obtained with 24 structurally different phosphorus and arsenic compounds show an average recovery of 99% and a mean standard deviation of ±1%. Excipients and diluents normally used in drug formulations do not interfere.

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Spektrophotometrische Bestimmung von Phosphor und Arsen in organischen Arzneimitteln

Zusammenfassung Eine einfache und genaue Methode zur Mikrobestimmung von Phosphor und Arsen in einigen organischen Arzneimitteln wurde angegeben. Sie beruht auf der Umsetzung des Phosphors zu Phosphat und des Arsens zu Arsenat sowie deren Fällung mit Chinolin und Natriummolybdat. Der Chinolinüberschuß wird spektrophotometrisch bei 312,5 nm in Ammonium-acetat bei pH 5,5 gemessen. Die mit 24 strukturell verschiedenen Phosphorbzw. Arsenverbindungen erhaltenen Resultate ergaben eine durchschnittliche Wiederfindungsrate von 99% und eine rel. Standardabweichung von ±1%. Arzneimittelträger und Verdünnungsmittel stören nicht.

     

Microdetermination of divalent sulphur in aliphatic compounds by visual titrimetry,potentiometry, and atomic absorption spectrometry

Summary Divalent sulphur in structurally different aliphatic compounds including thiols, sulphides, disulphides and thiocarbonyls is selectively determined by reaction with solid potassium hydroxide at 250–280° for 5–10 min, followed by addition of alkali plumbite whereby lead sulphide is stoichiometrically formed. The excess lead ions are measured by: (a) atomic absorption spectrometry at 217 nm; or (b) potentiometric titration with EDTA at pH 4.6 using the lead ion selective electrode; or (c) visual titration with EDTA using urotropine buffer and Xylenol Orange indicator. An average recovery of 99%, and a mean standard deviation of 0.9% are obtainable with samples down to 2 mg. Divalent sulphur in many aromatic compounds, and tetra- and hexa-valent sulphur in both aliphatic and aromatic compounds do not interfere.

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Mikrobestimmung von zweiwertigem Schwefel in aliphatischen Verbindungen durch visuelle Maanalyse, Potentiometrie und Atomabsorptionsspektrometrie

Zusammenfassung Zweiwertiger Schwefel in verschieden strukturierten aliphatischen Verbindungen wie Thiolen, Sulfiden, Disulfiden und Thiocarbonylverbindungen, lät sich durch Umsetzung mit festem Kaliumhydroxid bei 250–280° C durch 10 min und Zugabe von Alkaliplumbit bestimmen, wobei Bleisulfid in stöchiometrischer Menge gebildet wird. Der Überschuß an Bleiionen wird gemessen: a) durch Atomabsorptionsspektrometrie bei 217 nm; b) durch potentiometrische Titration mit ÄDTA bei pH 4,6 mit einer bleiionenspezifischen Elektrode; oder c) durch visuelle Titration mit ÄDTA, Urotropin als Puffer und Xylenolorange als Indikator. Ein durchschnittliches Ergebnis von 99% und eine mittlere Standardabweichung von 0,9% sind bei Einwaagen von wenigstens 2 mg erreichbar. Zweiwertiger Schwefel in vielen aromatischen Verbindungen, vier- und sechswertiger Schwefel sowohl in aliphatischen als auch in aromatischen Verbindungen stört nicht.

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Based on a paper presented at the Euroanalysis III Conference, Dublin, August 20–25, 1978.     

Hyperfine interaction experienced by181Ta nuclei at the Hf site in HfFe2−xSix compounds through a decoupling experiment

The time-differential perturbed angular correlation (TDPAC) experiments involving the 133–482 keV γ-γ cascade in¹⁸¹Ta have been performed in the presence of an external magnetic field along the quantization axis to measure the hyperfine magnetic field experienced by¹⁸¹Ta nuclei at the Hf site in the pseudobinary compounds HfFe_2?xSi_x with x=0.1 and x=0.3. The hyperfine magnetic fields measured at 298 K are H_hf=133.1±12.0 kG in the cubic (C15) Laves phase compound HfFe_1.9Si_0.1 and H_hf=76.8±7.0 kG in the hexagonal (C14) Laves phase compound HfFe_1.7Si_0.3. The measured hyperfine fields are discussed within the framework of the Campbell-Blandin model.