4- and 5-trifluoromethylimidazoles. Novel cyclization of trifluoroacetylated aldehyde dimethylhydrazones

Thermally induced cyclization reaction of trifluoroacetylated arylaldehyde dimethylhydrazones 1 in refluxing toluene afforded 1-methyl -4 -aryl -5 -trifluoromethylimidazoles 2 in good yields. In contrast thermal cyclization of 1 in the presence of silica gel gave regioisomeric 1-methyl -4 -trifluoromethyl -5 -aryl-imidazoles 5 as major products. These reactions could be extended to the syntheses of related several 1,4,5-trisubstituted imidazoles.     

Performance Characteristics of Power Build-Up Cavity for Raman Spectroscopic Measurement

Performance characteristics of power build-up cavity (PBC) as the light source of a Raman spectroscopy based gas sensor were studied. The key parameter to optimize stable and high intra-cavity power operation was beam diameter of the back reflected beam from external cavity to diode laser. The optimum diameter determined by an appropriate distance between the cavity and diode laser was found to be comparable with the waveguide cross section of diode laser for the effective spatial filtering, where inevitable cavity coupling loss caused by slight spatial mode mismatching existed. A PBC with a finesse of ∼10300 achieved a stable TEM₀₀ mode in excess of intra-cavity power of 80 watts pumped by a 10 milliwatts diode laser. Simultaneously, the PBC wavelength is found to be passively locked effectively at 670 +/− 0.15 nm where the center of the gain region exists. A Raman spectrum of nitrogen measurement was demonstrated.     

Disilane- and siloxane-bridged biphenyl and bithiophene derivatives as electron-transporting materials in OLEDs

Optical, electrochemical, and electron-transporting properties of disilane- and siloxane-bridged biphenyl and bithiophene derivatives were investigated, in comparison with those of the monosilane-bridged analogues (siloles). The UV spectra and cyclic voltammograms indicated that elongation of the silicon bridge suppresses the π-conjugation, in accordance with the results of DFT calculations. The DFT calculations indicated also that the disilane-bridged biphenyl and siloxane-bridged bithiophene should have the low-lying HOMOs and LUMOs. The electron-transporting properties were evaluated by the performance of triple-layered OLEDs having vapor-deposited films of the Si-bridged compound, Alq₃, and TPD, as the electron-transport, emitter, and hole-transport, respectively. Of these, the device with a disilane-bridged biphenyl exhibited the high performance with the maximum current density of 590 mA/cm² at the applied electric field of 12 × 10⁷ V/m (applied bias voltage = 13 V) and the maximum luminance of 22 000 cd/m² at 13 × 10⁷ V/m.     

Study of pyrolysis kinetic of green corn husk

In this paper, it was suggested the use of green corn husk, which is a biomass from agro-industry, as an alternative source of energy through its pyrolysis. Green corn husk characterization was done through immediate and elemental analysis of its components: cellulose, hemicelluloses, and lignin. It was also measured its higher calorific value. The pyrolysis study of green corn husk was done by the isoconversion and the Master plots method. Thermogravimetric plots were obtained at heating rates of 5, 10, 15, and 20 °C min^?1. The pyrolysis kinetics parameters were studied through the Flynn–Wall–Ozawa (FWO), Kissinger, and Friedman models. The Master plots method was used to determine the pyrolysis reaction order. The results of the reaction energy activation were found to be in the range 105.21–157.46 kJ mol^?1 by the FWO method, 150.50 kJ mol^?1 by the Kissinger method, and ranged 120.66–163.81 kJ mol^?1 by the Friedman method. The Master plots method showed a three-way-transport diffusional kinetics for the biomass de-volatilization process. The higher calorific value found for green corn husk was 16.14 MJ kg^?1. The simulation showed correlation between the experimental data and the proposed model for conversion values up to 0.8.

     

Synthesis and characterization of a novel phosphorus–nitrogen‐containing flame retardant and its application for textile

The economic and environmentally friendly flame‐retardant compound, tetramethyl (6‐chloro‐1,3,5‐triazine‐2,4‐diyl)bis(oxy)bis(methylene) diphosphonate ( CN‐1 ), was synthesized by a simple two‐step procedure from dimethyl phosphate, and its chemical structure was characterized by ¹H, ¹³C, and ³¹P nuclear magnetic resonance and gas chromatography mass spectroscopy. Using the traditional pad–dry–cure method, we obtained several different add‐ons (wt%) by treating cotton twill fabric with flame retardant ( CN‐1 ). Thermogravimetric analysis, in an air and nitrogen atmosphere, of the modified cotton showed that decomposition occurred ~230°C with 16% residue weight char yield at 600°C, indicating high thermal stability for all treated levels. Limiting oxygen index (LOI) and the vertical flammability test were employed to determine the effectiveness of the flame‐retardant treatments on the fabrics. LOI values increased from ~18 vol% oxygen in nitrogen for untreated fabric to maximum of 34 vol% for the highest treatment level. Fabrics with higher levels of flame retardant also easily passed the vertical flammability test. Furthermore, Fourier transform infrared and scanning electron microscopy were utilized to characterize the chemical structure as well as the surface morphology of the flame‐retardant treated twill fabrics, including char area and the edge between unburned fabric and char area. Copyright © 2011 John Wiley & Sons, Ltd.     

Flow injection on-line minicolumn preconcentration and determination of trace copper ions using an alumina/titanium oxide grafted silica matrix and FAAS

We describe the analytical performance of a hybrid material composed of SiO₂, Al₂O₃ and TiO₂. It was prepared by a sol–gel process and can act as an adsorbent in the continuous-flow enrichment of copper. A minicolumn was packed with the material, copper ions are adsorbed at pH 9.13, then eluted with 1.0?mol?L^?1 nitric acid, and determined by FAAS. The material was characterized by infrared spectroscopy, scanning electron and energy dispersive spectroscopy, energy dispersive X-ray fluorescence analysis, powder X-ray diffraction, and specific surface area analysis. No significant interference was observed for most ions in up to copper/interferent ratios of 1:100 and of 1:500 in case of Ca(II), Ba(II), and Mg(II). The breakthrough capacity is 1.4?mg?g^?1 under dynamic conditions. The limits of detection and of quantification are 0.50 and 1.4?μg?L^?1, respectively, and the calibration plot is linear in the range from 5.0 to 245.0?μg?L^?1 (r?=?0.999). The relative standard deviation is 3.20 (for n?=?7 and at a Cu(II) concentration of 10?μg?L^?1). The method was applied to the determination of trace copper ions in water, vegetable and alcohol fuel samples.