A sensitive and efficient method for trace analysis of some phenolic compounds using simultaneous derivatization and air‐assisted liquid–liquid microextraction from human urine and plasma samples followed by gas chromatography–nitrogen phosphorous detection

In present study, a simultaneous derivatization and air‐assisted liquid–liquid microextraction method combined with gas chromatography–nitrogen phosphorous detection has been developed for the determination of some phenolic compounds in biological samples. The analytes are derivatized and extracted simultaneously by a fast reaction with 1‐flouro‐2,4‐dinitrobenzene under mild conditions. Under optimal conditions low limits of detection in the range of 0.05–0.34 ng mL^?1 are achievable. The obtained extraction recoveries are between 84 and 97% and the relative standard deviations are less than 7.2% for intraday (n = 6) and interday (n = 4) precisions. The proposed method was demonstrated to be a simple and efficient method for the analysis of phenols in biological samples. Copyright © 2015 John Wiley & Sons, Ltd.     

大学物理课程网络辅助教学系统的构建与应用

本文介绍了上海交通大学大学物理课程网络辅助教学系统的设计思想、整体结构和主要的功能模块，概述了运用网络辅助教学系统实施“课堂教学＋网络辅助教学”：这种教学模式的应用情况．     

Magnetic properties of mechanically alloyed Co–Ti powder

An amorphous phase containing traces of non-transformed Co and Ti powders was obtained by mechanical alloying nominal compositions of Co₆₇Ti₃₃ and Co₅₀Ti₅₀ in a high-energy ball-mill. These alloys were prepared from elemental powders of Co and Ti. The heat treatment of Co₆₇Ti₃₃ at 573, 873 and 1173 K crystallized nanoparticles of Co₂Ti and Co₃Ti compounds, while the same treatments conducted on Co₅₀Ti₅₀ resulted in the formation of Co₂Ti and CoTi nanoparticles. The saturation magnetizations reached a maximum value in the amorphous state and they decreased when the temperatures of the heat treatment rose. Demagnetizing interparticle interaction effects were estimated through hysteresis loops and initial magnetization curves using the Fourier technique.     

Microstructure and high-temperature wear resistance of a laser surface alloyed γ-TiAl with carbon

TiC reinforced composite coating on γ-TiAl alloy was successfully fabricated by laser surface alloying with carbon. The fine TiC reinforcing phase had a gradient distribution in the coating, and its growth morphology of TiC in laser surface alloyed coating was in unique faceted platelet-like. The composite coating exhibited high hardness and excellent high-temperature sliding wear resistance.     

Photoluminescence of Ge(Si)/Si(0 0 1) self-assembled islands in the near infra-red wavelength range

The dependence of photoluminescence spectra of structures with GeSi/Si(0 0 1) self-assembled nanoislands on growth temperature has been investigated. It was shown that the redshift of the island-related photoluminescence peak with a decrease of the growth temperature is associated with suppression of Si diffusion in the islands and an increase of Ge content in them. For the first time a photoluminescence signal from SiGe islands was observed at energies much lower than the Ge band gap. The energy position of the island-related photoluminescence peak is well described by the model of optical transition, which is indirect in real space. The photoluminescence signal at 1.55 μm from GeSi/Si(0 0 1) self-assembled islands was obtained up to room temperature.     

Coexisting antiferromagnetism and ferromagnetism in mechanically alloyed Fe-rich Fe–Ni alloys: implications regarding the Fe–Ni phase diagram below 400°C

Fe–Ni alloys below the Invar region with compositions Fe_100−xNi_x (x=21, 24, and 27 at%) were prepared by high-energy ball milling technique (mechanical alloying). The as-milled samples, characterized by X-ray diffraction and Mössbauer spectroscopy, contain a mixture of (BCC) and γ (FCC) phases, whereas the samples annealed at 650°C for 0.5 h show a single γ (FCC) phase displaying a single line Mössbauer spectrum at room temperature (RT). At low temperature, the Mössbauer spectra of annealed Fe₇₆Ni₂₄ and Fe₇₃Ni₂₇ alloys show the existence of a magnetically split pattern together with a broad singlet, which are ascribed to a high-moment ferromagnetic Ni-rich phase and a low-moment Fe-rich phase, respectively. The Fe-rich phase in annealed Fe₇₆Ni₂₄ alloy, which is paramagnetic at RT, undergoes antiferromagnetic ordering at 40 K, estimated from the dramatic line broadening of its spectrum, giving rise to a small hyperfine field (e.g. 2 T at 6 K). The coexistence of these phases is attributed to phase segregation occurring in these alloys as a result of enhanced atomic diffusion. The stability of these alloys towards martensitic (FCC→BCC) transformation at low temperatures is discussed in connection with the Fe–Ni phase diagram below 400°C.     

Matrix assisted pulsed laser evaporation processing of triacetate-pullulan polysaccharide thin films for drug delivery systems

We report the first successful deposition of triacetate-pullulan polysaccharide thin films by matrix assisted pulsed laser evaporation. We used a KrF* excimer laser source (λ = 248 nm, τ ≈ 20 ns) operated at a repetition rate of 10 Hz. We demonstrated by FTIR that our thin films are composed of triacetate-pullulan maintaining its chemical structure and functionality. The dependence on incident laser fluence of the induced surface morphology is analysed.     

Mechanical alloying of a thermoelectric alloy: Pb0.65Sn0.35Te

We report in this paper a study of the mechanical alloying (MA) process for the Pb_0.65Sn_0.35Te alloy. MA has been carried out in a high-energy planetary ball mill. The mechanism of formation has been studied from systematic analyses of mechanically alloyed powders using X-ray diffraction, differential scanning calorimetry and scanning electron microscopy. As it was already observed for the MA of PbTe, this synthesis is associated with an exothermic reaction between the elemental powders. The required time to reach an homogeneous phase Pb_0..65Sn_0.35Te is 31 h.     

Mass spectrometric analysis of low molecular mass polyesters by laser desorption/ionization on porous silicon

A low molecular mass polyester was analyzed by desorption/ionization on porous silicon (DIOS) mass spectrometry. The results were compared with those of matrix-assisted laser desorption ionization (MALDI) mass spectrometry using matrixes of alpha-cyano-4-hydroxycinnamic acid (CHCA) and 10,15,20-tetrakis(pentafluorophenyl)porphyrin (F20TPP). The CHCA matrix was not suitable for characterization of low molecular mass components of the polyester because the matrix-related ions interfered with the component ions. On the other hand, the F20TPP matrix showed no interference because no matrix-related ions appeared below m/z 822. However, the solvent selection for determining optimal conditions of sample preparation was limited, because F20TPP does not dissolve readily in any of the available organic solvents. In the DIOS spectra, the polymer ions were observed at high sensitivity without a contaminating ion. No matrix is needed for DIOS spectra of low molecular mass polyesters, facilitating sample preparation and selectivity of a precursor ion in post-source decay measurements.     

Do intramolecular halogen bonds exist? Ab initio calculations and crystal structures’ evidences

Cl···O intramolecular contacts are analysed here. Hence the Cambridge Structural Database (CSD) search was performed to find five-membered Cl–C=C–C=O pseudo-rings closed through Cl···O intramolecular contacts. Such rings were analysed and it was found that some of Cl···O distances are smaller than the corresponding sum of van der Waals radii. Additionally ab initio MP2/6-311++G(d,p) calculations and AIM analyses were carried out here on 3-chloropropenal and its fluoro derivatives to deepen the nature of intramolecular Cl···O interactions, some of findings may indicate that they are attractive and stabilizing ones. This paper is dedicated to Prof. T. M. Krygowski on the occasion of his 70th birthday