135 resultados para 030200 INORGANIC CHEMISTRY


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A novel organic-inorganic hybrid complex [(CuCl)(2) (o-phen)](infinity) 1 (o-phen = o-phenanthroline) has been hydrothermally synthesized and structurally characterized by elemental analyses, XPS spectrum, TG analysis, and single-crystal X-ray diffraction. Compound I crystallizes in the monoclinic system, space group P2(1)/n, a = 3.7285(7) Angstrom, b = 19.603(4) Angstrom, c = 16.757(3) Angstrom, beta = 95.83(3)degrees, V = 1218.4(4) Angstrom(3), Z = 4, lambda(MoKalpha) = 0.71073 Angstrom (R(F) = 0.0643 for 2559 reflections). Data were collected on an R-axis RAPID diffractometer at 293 K in the range of 1.60 < θ < 27.48degrees. The title compound exhibits a one-dimensional chain-like scaffolding constructed by the unusual [Cu3Cl3] hexagon motifs by, sharing opposite edges. Only Cu(1) sites of the [Cu3Cl3] hexagon are coordinated with N donors of o-phen groups. Furthermore, the three-dimensional supermolecular architecture is formed by C-H...Cl hydrogen bonds between o-phen groups and CuCl chains.

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We have employed several techniques, including cyclic voltammetry, UV-Vis spectrometry, small-angle X-ray diffraction, X-ray photoelectron spectroscopy and electrochemical impedance spectroscopy, to characterize the formation processes and interfacial features of ultrathin multilayer films of silicotungstate and a cationic redox polymer on cysteamine-coated Au electrodes self-assembled monolayers. All of these techniques confirm that the multilayer films are built up stepwise as well as uniformly in a layer-by-layer fashion. In particular, the electrochemical impedance spectroscopy is successfully used to monitor the multilayer deposition processes. It has been proved that the electrochemical impedance spectroscopy is a very useful technique in characterization of multilayer films because it provides valuable information about the interfacial impedance features.

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A novel organic-inorganic hybrid vanadium oxide [V4O10(o-phen)(2)], involving all vanadium atoms present in +5 oxidation, has been hydrothermally synthesized and characterized by elemental analysis, IR, UV-vis, ESR, XPS spectra and TG-DTA thermal analysis. The single-crystal X-ray diffraction shows that the red-brown crystal is formed in the triclinic system, space group P (1) over bar, a = 9.782(2), b = 6.5124(14), c = 19.765(4) Angstrom, alpha = 89.94(2)degrees, beta = 100.66(2)degrees, gamma = 89.86(2)degrees. The title compound exhibits an infinite one-dimensional ladder-type tetravanadate skeleton with organonitrogen donors of o-phenanthroline ligands coordinated directly to the vanadium oxide framework.

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Photoluminescent organic-inorganic composite films incorporating the rare-earth-containing polyoxometalate Na-9[EuW10O36] (EW) and poly(allylamine hydrochloride) (PAH) have been prepared by the layer-by-layer self-assembly method. UV-vis spectroscopy and ellipsometry were used to follow the fabrication process of the EW/PAH composite films. The experimental results show that the deposition process is linear and highly reproducible from layer to layer. An average EW/PAH bilayer thickness of ca. 2.1 nm was determined by ellipsometry. In addition, scanning electron microscopy and atomic force microscopy images of the EW/PAH composite films indicate that the film surface is relatively uniform and smooth. The photoluminescent properties of these films were investigated by fluorescence spectroscopy.

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A nanoparticulate ferric oxide-copper tris(2,4-di-tert-amylphenoxy)-8-quinolinolylphthalocyanine hybrid ultrathin film was constructed from alternate layers by the Langmuir-Blodgett technique. The composition, morphology and structure of the film were studied by X-ray photoelectron spectroscopy (XPS), transmission electron microscopy, atomic force microscopy, small-angle X-ray diffraction, visible spectroscopy and polarized UV-Vis spectroscopy. All the above analyses suggest that the thin film is a kind of one-dimensional superlattice, composed of organic and inorganic components. The XPS data reveal that the nanoparticulate ferric oxide exists as an alpha-Fe2O3 phase in the films. Gas-sensing measurements show that the hybrid LB film has very fast response-recovery characteristics towards 2 ppm C2H5OH vapor.

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A novel organic-inorganic hybrid compound {[Cu (2, 2'-bpy)(2)](2)Mo8O26} has been hydrothermally Synthesized and structurally characterized by single-crystal X-ray diffraction. The compound crystallizes in the orthorhombic space group, Pna2(1), with a=2.4164 (5), b=1.8281 (4), c=1.1877 (2) nm, V=5.247(2) nm(3), Z=4, and final R-1=0.0331, wR(2)=0.0727. The structure consists of discrete {[Cu(2,2'-bpy)(2)](2)Mo8O26} clusters, constructed from a beta -octamolybdate subunit[Mo8O26](4-) covalently bonded to two [Cu(2,2'-bpy)(2)](2+) coordination complex cations via bridging oxo groups. In addition, the spectroscopic properties and thermal behavior of this compound have been investigated by spectroscopic techniques (UV-vis, IR, Raman and EPR spectra) and TG analysis.

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The structural relaxation process of an inorganic glass (Li(2)O2SiO(2)) has been studied by differential scanning calorimetry. The sample is subjected to different thermal ageing histories with isothermal stages at an ageing temperature of T-g - 30 degrees C for different ageing times and at an ageing time of 16 h for different ageing temperatures. A four-parameter Tool-Narayanaswamy-Moynihan (TNM) model, is applied to simulate the normalized specific-heat curves measured. The ageing-temperature and ageing-time dependence of the structural relaxation parameters in the TNM model is obtained. (C) 1998 Elsevier Science S.A. All rights reserved.

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A new type of sol-gel organic-inorganic hybrid material was developed and used for the production of biosensors. This material is composed of silica sol and a grafting copolymer of poly(vinyl alcohol) with 4-vinylpyridine. It prevents the cracking of conventional sol-gel-derived glasses and eliminates the swelling of the hydrogel. The optimum composition of the hybrid material was first examined, and then glucose oxidase was immobilized in this matrix to demonstrate its application. The characteristics of the biosensor were studied by cyclic voltammetry and chronoamperometry. The biosensor exhibited a series of good properties: high sensitivity (600 nA mmol(-1)L(-1)), short response time (11 s) and remarkable long-term stability in storage (at least 5 months). In addition, the characteristics of the second-generation biosensor with the use of tetrathiafulvalene as a mediator mere discussed.

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The structural relaxation process of an inorganic glass (Li2O . 2SiO(2)) at an ageing temperature of 703 K for an ageing time of 1 h has been studied by differential scanning calorimetry. A four-parameter model-the Tool-Narayanaswamy-Moynihan (TNM)-model was applied to simulate the normalized specific heat curve measured. A set of optimized parameters, Delta h*/R,beta,InA, and x was obtained. Then the effects of variation of each adjustable parameter on the calculated specific heat were summarized. (C) 1997 Elsevier Science S.A.

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Marine sediment is the important sources and sinks of carbon. The inorganic carbon(IC) in marine sediments plays an important role in carbon cycling. In order to understand IC function in carbon cycling, sequential extraction method based on IC combined chemical strength difference were established to get five phases: NaCl phase (step I), NH3 - H2O phase (step II), NaOH phase (step III), NH2OH . HCl phase (step IV) and HCl phase(step V). The best extraction conditions were obtained by a series of experiments. Extractants were added into plastic centrifuge tubes in Step I - M, the capped tube were placed on a shaker table to keep the solids suspended for two hours. The suspended solution was separated by centrifugal, the residues were washed with water. The two supernatant were combined and the CO, was finally determined by volumetric analysis. The residues were transferred into conical flask in step IV and V, and then the extractants were added. The produced CO2 was adsorbed by saturated Ba(OH)(2) solution, and determined by volumetric analysis. This method for IC has a good precision in the analysis sediment samples.

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Dissolved inorganic carbon (DIC) account for more than 95% of total carbon in seawater, so it is necessary to make reliable and precise measurements of DIC to study marine carbon cycling. In order to establish a simple and speed method, an airproof device of gas extraction-absorption was designed. Finally a simple method was developed for the determination of DIC in seawater through a large mount of experiments. The determination procedure is as follows: 100 similar to 150 mL seawater was put into conical flask, then add 10% H3PO4, the DIC in seawater sample was dissolved to form CO2 gas and carried by pure N-2, then the CO2 gas was absorbed by two grades 0.1 mol/L NaOH solution. Finally the absorbed solution was titrated by HCl standard solution of 0.01000 mol/L with the end points detected with the indicator phenolphthalein and bromocresol green-methyl red mixture. The precision and accuracy of the method were satisfied. This method was used to analyse seawater samples from Jiaozhou bay in June, 2003. The result shows that the average DIC in surface seawater is 2066 mumol/L, DIC in bottom seawater is 2075 mumol/L inside bay, but the average DIC in surface seawater is 1949 mumol/L, DIC in bottom seawater is 2147 mumol/L outside bay.

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Nine novel triazole compounds containing ester group were designed and synthesized. Their structures were confirmed by elemental, H-1 NMR and IR analyses, and optimized by means of DFT (Density Functional Theory) method at the B3LYP/6-31G* level. Based on the quantum-chemical calculation results and the Pearson coefficients between FA and quantumchemical parameters, V, LogP, MR and E-HOMO are shown to be the important relative factors which affect FA of the title compounds.