167 resultados para ESI-MS characterization


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Thiazolyl heterocyclic azo dye and its metal (Ni2+, Co2+)-azo complexes were synthesized. Their structures were confirmed by elemental analysis, UV-VIS absorption spectra, FT-IR, H-1 NMR and MALDI-MS. The thermal properties of metal complexes were studied by DSC-TGA. The optical constants (complex refractive index N=n + ik) and thickness of the complex thin films on polished single-crystal silicon substrates were investigated on a scanning ellipsometer. Results indicate that thiazolyl metal-azo complexes possess good optical and thermal properties. They would be a promising recording medium candidate for NVD with the Super-resolution near field structure (Super-RENS) technology. (c) 2007 Elsevier B.V. All rights reserved.

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The spectrum properties of transparent (Nd0.01Y0.94La0.05)(2)O-3 ceramics were investigated. It was found that all absorption bands of (Nd0.01Y0.94La0.05)(2)O-3 ceramics are broadened, of which the full width at half maximum of the peak centered at 804 nm is 8 nm and its absorption cross section is 1.02x10(-20) cm(2). The emission cross section of (Nd0.01Y0.94La0.05)(2)O-3 ceramics located at 1078 nm is 5.71x10(-20) cm(2) and its fluorescent lifetime is 0.214 ms, which are similar to those of 1.0 at. %Nd:Y2O3 ceramics. These indicate that (Nd0.01Y0.94La0.05)(2)O-3 transparent ceramics has excellent spectroscopic properties.

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Continuous gradient elution chromatography (CGEC) was employed to purify and separate enzymes and polysaccharides from the sap of Rhus vernicifera Chinese lacquer tree. There are three different molecules with laccase enzyme activity. Two are enzymes of each other (L1, and L2), whereas the third (RL) is an entirely separate entity. Two polysaccharides (GP1 and GP2) were also found. The Rhus laccase (RL), and isoenzymes L1 and L2, have peak molecular masses of 109,100, 120,000, 103,000 respectively; each has four copper atoms per molecule, and the pI values were 8.2, 8.6, and 9.1, respectively. The structure of the laccases was studied by Fourier-transform infrared (FT-IR) and Matrix-assisted laser desorption/ionization time-of flight (MALDI-TOF) mass spectrometry. The typical amide I (1646 cm(-1)) and amide II (1545 cm(-1)) bands were observed. The results from MALDI-TOF were similar to those from CGEC, but the molecular mass from the MALDI-TOF was significantly different from that obtained from sodium dodecyl sulfate polyacrylamide gel electrophoresis (SDS-PAGE). (c) 2006 Elsevier B.V. All rights reserved.

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A new AlGaN/AlN/GaN high electron mobility transistor (HEMT) structure using a compositionally step-graded AlGaN barrier layer is grown on sapphire by metalorganic chemical vapour deposition (MOCVD). The structure demonstrates significant enhancement of two-dimensional electron gas (2DEG) mobility and smooth surface morphology compared with the conventional HEMT structure with high Al composition AlGaN barrier. The high 2DEG mobility of 1806 cm(2)/Vs at room temperature and low rms surface roughness of 0.220 nm for a scan area of 5 mu m x 5 mu m are attributed to the improvement of interfacial and crystal quality by employing the step-graded barrier to accommodate the large lattice mismatch stress. The 2DEG sheet density is independent of the measurement temperature, showing the excellent 2DEG confinement of the step-graded structure. A low average sheet resistance of 314.5 Omega/square, with a good resistance uniformity of 0.68%, is also obtained across the 50 mm epilayer wafer. HEMT devices are successfully fabricated using this material structure, which exhibits a maximum extrinsic transconductance of 218 mS/mm and a maximum drain current density of 800 mA/mm.

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AlGaN/GaN high electron mobility transistor (HEMT) structures were grown on 2 inch sapphire substrates by MOCVD, and 0.8-mu m gate length devices were fabricated and measured. It is shown by resistance mapping that the HEMT structures have an average sheet resistance of approximately 380 Omega/sq with a uniformity of more than 96%. The 1-mm gate width devices using the materials yielded a pulsed drain current of 784 mA/mm at V-gs=0.5 V and V-ds=7 V with an extrinsic transconductance of 200 mS/mm. A 20-GHz unity current gain cutoff frequency (f(T)) and a 28-GHz maximum oscillation frequency (f(max)) were obtained. The device with a 0.6-mm gate width yielded a total output power of 2.0 W/mm (power density of 3.33 W/mm) with 41% power added efficiency (PAE) at 4 GHz.

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Methomyl, an extremely toxic pesticide, is widely used in agriculture. A strain named mdw-1 capable of degrading methomyl rapidly was successfully isolated from activated sludge in this study. It could utilize methomyl as the sole carbon or nitrogen source. The optimal temperature and medium pH for its growth and methomyl biodegradation were 30 degrees C and 7.0, respectively. It was identified as a Paracoccus sp. according to its morphological features, physiological and biochemical characteristics, and phylogenetic analysis based on the sequence of 16S rDNA. Gas chromatography-mass spectrometry (GC-MS) analysis showed that methomyl could be completely transformed to S-methyl-N-hydroxythioacetamidate in 10 h of incubation with the isolate mdw-1.

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GaAs epilayers grown on Si by metalorganic chemical vapor deposition (MOCVD) using an ultrathin a-Si buffer layer were characterized by deep-level transient spectroscopy (DLTS). Six electron traps with activation energies of 0.79, 0.67, 0.61, 0.55, 0.53 and 0.32 eV below the conduction band were determined by fitting the experimental spectra. Two of the levels, C (0.61 eV) and F (0.32 eV), were first detected in GaAs epilayers on Si and identified as the metastable defects M3 and M4, respectively. In order to improve the quality of GaAs/Si epilayers, another GaAs layer was grown on the GaAs/Si epilayers grown using MOCVD. The deep levels in this regrown GaAs epilayer were also studied using DLTS. Only the EL2 level was found in the regrown GaAs epilayers. These results show that the quality of the GaAs epilayer was greatly improved by applying this growth process.

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Gas chromatography-mass spectrometry with electron ionization and positive-ion chemical ionization and comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC x GC-TOF-MS) were applied for the characterization of the chemical composition of complex hydrocarbons in the non-polar neutral fraction of cigarette smoke condensates. Automated data processing by TOF-MS software combined with structured chromatograms and manual review of library hits were used to assign the components from GC x GC-TOF-MS analysis. The distributions of aliphatic hydrocarbons and aromatics were also investigated. Over 100 isoprenoid hydrocarbons were detected, including carotene degradation products, phytadiene isomers and carbocyclic diterpenoids. A total of 1800 hydrocarbons were tentatively identified, including aliphatic hydrocarbons, aromatics, and isoprenoid hydrocarbons. The identified hydrocarbons by GC x GC-TOF-MS were far more than those by GC-MS. (C) 2004 Elsevier B.V. All rights reserved.

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The electrospray ionization ion trap multiple-stage tandem mass spectrometry (ESI-MSn) and electrospray ionization Fourier transform ion cyclotron resonance multiple-stage tandem mass spectrometry (ESI-FT-ICR-MSn) have been applied successfully to the direct investigation of a number of dibenzocyclooctadiene lignan constituents from the methanol extracts of the Fructus Schisandrae in the positive ion mode. The detailed structural characterization of the same skeleton and different peripheral substituents had been studied and the precise elemental compositions of ions at high mass resolution had been obtained. So the fragmentation mechanisms could be clarified.

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Seven compounds, four flavones and three triterpenoids from Glycyrrhiza uralensis Fisch. extract are identified by high performance liquid chromatography coupled with electrospray ionization multi-tandem mass spectrometry (HPLC-ESI-MSn). The fragmentation pathways of these compounds are investigated by ESI-MSn and Fourier transform ion cyclotron resonance multiple-stage tandem mass spectrometry (FT-ICR-MSn). Comparing the retention times (t(R)) and mass spectra with those of reference compounds, seven components are identified in Glycyrrhiza uralensis Fisch. and their MSn data proposed plausible schemes for their fragmentation. All the experimental results show that ESI-MSn and FT-ICR-MSn are powerful tools for the structural characterization of triterpenoids and flavones

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Monodisperse, core-shell-structured SiO2@NaGd(WO4)(2):Eu3+ particles were prepared by the sol-gel method. The samples were characterized by X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, photoluminescence (PL), and low-voltage cathodoluminescence (CL) as well as time-resolved PL spectra and lifetimes. PL and CL study revealed that the core-shell-structured SiO2@NaGd (WO4)(2):Eu3+ particles show strong red emission dominated by the D-5(0) - F-7(2) transition of Eu3+ at 614 nm with a lifetime of 0.74 ms. The PL and CL emission intensity can be tuned by the coating number of NaGd(WO4)(2):Eu3+ phosphor layers on SiO2 and by accelerating voltage and the filament current, respectively.

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The non-covalent complexes between three flavonoid glycosides (quercitrin, hyperoside and rutin) and heptakis(2,6-di-O-methyl)-beta-cyclodextrin (DM-beta-CD) were investigated by electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry (ESI-FTICR-MS). The 1:1 complexation of each flavonoid glycoside (guest) to the DM-beta-CD (host) was monitored in the negative ion mode by mixing each guest with an up to 30-fold molar excess of the host. The binding constants for all complexes were calculated by a linear equation in the order: DM-beta-CD:quercitrin > DM-beta-CD:rutin > DM-beta-CD:hyperoside. A binding model for the complexes has also been proposed based on the binding constants and tandem mass spectrometric data of these complexes.

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A new straightforward strategy for synthesis of novel hyperbranched poly (ether amide)s from readily available monomers has been developed. By optimizing the reaction conditions, the AB(2)-type monomers were formed dominantly during the initial reaction stage. Without any purification, the AB(2) intermediate was subjected to further polymerization in the presence (or absence) of an initiator, to prepare the hyperbranched polymer-bearing multihydroxyl end-groups. The influence of monomer, initiator, and solvent on polymerization and the molecular weight (MW) of the resultant polymers was studied thoroughly. The MALDI-TOF MS of the polymers indicated that the polymerization proceeded in the proposed way. Analyses of H-1 NMR and C-13 NMR spectra revealed the branched structures of the polymers obtained. These polymers exhibit high-moderate MWs and broad MW distributions determined by gel permeation chromatography (GPC) in combination with triple detectors, including refractive index, light scattering, and viscosity detectors. In addition, the examination of the solution behavior of these polymers showed that the values of intrinsic viscosity [eta] and the Mark-Houwink exponent a were remarkably lower compared with their linear analogs, because of their branched nature.

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According to the strong application background of bioflavonoid and metal-flavonoid complexes, novel electrospray ionization tandem mass spectrometry (ESI-MSn) was applied to investigate the structure and fragmentation mechanism of transition metal-rutin complexes. In the full-scan mass spectra, different stoichiometric ratios of rutin-metal complexes were found. In the reaction between rutin and Cu, four kinds of complexes with four different stoichiometric ratios were produced. In the reaction between rutin and Zn, Mn(II), and Fe(II), only two kind of complexes with stoichiometric ratios of 1:1 and 1:2 occured. In further tandem mass spectrometric experiments of different rutin-metal complexes, product fragments, came from the neutral loss of the external rhamnose and the internal glucose unit, oligosaccharide chain, aglycone, and small organic molecules. According to the MSn data, we proposed a mechanism for all fragments of the rutin-Cu complex A and the structure of two rutin-Cu complexes, C and D.

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A series of cyclic (arylene phosphonate) oligomers were prepared by reaction of phenylphosphonic dichloride (PPD) with various bisphenols under pseudo-high dilution conditions via interfacial polycondensation. The yield of cyclic (arylene phosphonate) oligomers is over 85% by using hexadecyltrimethylammonium bromide as phase transfer catalyst (PTC) at 0 degreesC. The structures of the cyclic oligomers were confirmed by a combination of matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) and IR analysis. These cyclic oligomers undergo facile ring-opening polymerization in the melt by using potassium 4,4'-biphenoxide as the initiator to give linear polyphosphonate. Free-radical ring-opening polymerization of cyclic(arylene phosphonate) oligomers containing sulfur linkages was also performed in the melt using 2,2'-dithiobis(benzothiazole) (DTB) as the initiator at 270degreesC and the resulting polymer had a M-w of 8 x 10(3) with a molecular weight distribution of 4. Ring-opening copolymerization of these cyclic oligomers with cyclic carbonate oligomers was also achieved. The average molecular weight of the resulting copolymer is higher than the corresponding, homopolymer and the thermal stability of the copolymer is better than the corresponding homopolymer.