Investigation on Ochratoxin A stability using different extraction techniques

The stability of Ochratoxin A during its extraction using different extraction techniques has been evaluated. Microwave-assisted extraction and pressurised liquid extraction, in addition to two other reference methods of extraction, i.e. ultrasound-assisted and magnetic stirring-assisted extraction, were evaluated. The effect of extraction temperature using the cited techniques was checked.The results show that Ochratoxin A can be extracted using microwave-assisted extraction at temperatures up to 150 °C without degradation. Pressurised liquid extraction can be used at temperatures up to 100 °C, for extraction times of less than 30 min. Further, both ultrasound-assisted extraction and magnetic stirring extraction can be applied at temperatures up to 65 °C.High-performance liquid chromatography combined with fluorescence detection using a Chromolith RP-18e column at a flow rate of 5 mL min⁻¹ was used to quantify the Ochratoxin A. The retention time for the Ochratoxin A was 1.3 min. The limits of detection (LOD) and of quantification (LOQ) were 0.03 and 0.10 μg L⁻¹, respectively.     

Quantification of trace elements in human serum fractions by liquid chromatography and inductively coupled plasma mass spectrometry

On‐line coupling of LC and ICP‐MS has been used for fractionation and detection of species of Cu, Fe, I, Se and Zn in human serum. It has been shown that anion exchange chromatography provided better separation capability (both intra‐ and inter‐element) than size‐exclusion chromatography. The mobile phases for ion exchange chromatography consisted of Tris–HNO₃ buffer and ammonium salt (nitrate, acetate or formate). Formate was found to be the best mobile phase counter ion, enabling good chromatographic separation, and is acceptable for mass spectrometry too. The quantitative evaluation of element concentrations adhering to individual fractions was performed by the peak area normalization method. The repeatability of results ranged from 3 to 15% (depending on the element concentration level) and represented the main part of the result uncertainty. The accuracy of Cu and Zn fraction determinations was confirmed by comparison with the isotope dilution technique. Copyright © 2006 John Wiley & Sons, Ltd.     

倾斜下降管气液两相分层流截面含气率的计算与液层高度的预测

分层流是气液两相流中常见的流动型式，分层流中液层高度是计算的基本数据，由于界面波的存在，对液层的测量和预测都很困难．Ｖｌａｃｈｏｓ提出了预测气液两相分层流液层厚度的关系式，但这一关系式并不适用于倾斜下降管气液两相流．本文提出了计算倾斜下降管气液两相分层流截面含气率的理论模型，在这种模型下得到的截面含气率和实验结果符合良好．在大量实验的基础上，考虑了倾角、管径、气液各相折算速度的影响，根据实验数据提出了预测液层厚度的关系式。     

Si衬底上ZnSe外延膜的低压MOCVD生长

以硒化氢（H2Se）和二甲基锌为源材料，生长温度是300℃时，用低压金属有机化学气相沉积（LP－MOCVD）系统在Si(111)衬底上外延生长了ZnSe薄膜。通过X射线衍射（XRD）、扫描电子显微镜的能量色散（EDS）以及光致发光（PL）实验验证ZnSe外延膜的质量，在X射线衍射谱中只有一个强的ZnSe(111)面衍射峰，这说明外延膜是（111）取向的单晶薄膜，在能量色散谱中除了Si,Zn和Se原子外，没有观测到其他原子，说明ZnSe外延膜中杂质含量较少。ZnSe外延膜中Zn/Se原子比接近1，有较好的化学配比。在ZnSe外延膜的77K光致发光谱中没有观测到与深中心发射相关的发光峰，表明ZnSe外延膜的晶格缺陷密度较小。77K时的近带边发射峰447nm在室温时移至465nm附近。     

简析"静止液体内部压强公式验证"实验的设计策略

“静止液体内部压强公式验证”在现行教材中有两种实验方法。通过分析实验的设计策略，说明其作用、效果及操作上的困难，指出合理的与不合理诸因素，从而提出改进实验的方法，化难为易，提高实验教学效果。     

Influence of SiO2 in SiCp on the microstructure and impact strength of Al/SiCp composites fabricated by pressureless infiltration

The effect of SiO₂ in SiC_p and the following processing parameters on the microstructure and impact strength of Al/SiC_p composites fabricated by pressureless infiltration was investigated: Mg content in the aluminum alloy, SiC particle size, and holding time. Preforms of SiC_p in the form of rectangular bars (10 × 1 × 1 cm) were infiltrated at 1150°C in an argon→nitrogen atmosphere for 45 and 60 min by utilizing two aluminum alloys (Al-6 Mg-11 Si and Al-9 Mg-11 Si, wt.%). The results obtained show that the presence of SiO₂ in SiC affects the microstructure and impact strength of the composites significantly. When Al₄C₃ is formed, the impact strength decreases. However, a high proportion of SiC to SiO₂ limits the formation of the unwanted Al₄C₃ phase in the composites. Also, a higher content of Mg in the Al alloy lowers the residual porosity and, consequently, increases the composite strength. The impact strength grows with decrease in SiC particle size and increases considerably when the residual porosity is less than 1%. Russian translation published in Mekhanika Kompozitnykh Materialov, Vol. 42, No. 3, pp. 401–418, May–June, 2006.     

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.     

Localized bifurcations and defect instabilities in the convection of a nematic liquid crystal

The stationary and the time-dependent homogeneous ordered states in convection may both become unstable against localized perturbations. Defects are then created and they may contribute to the disorganization of the homogeneous state. We present an experimental study of defects in some homogeneous stationary structures as well as in the traveling-wave states of convection of a nematic liquid crystal. We show that the core of the defects is a germ of the unstable state and it can become unstable under the external stress. Then, either fully homogeneous states with the symmetry of the core, or complex disordered states can develop from the local instability of defects in processes quite similar to displacive transitions in solids. Some of the main features are qualitatively similar to numerical simulations of an appropriate Landau-Ginzburg equation.     

La5Al3Ni2 – an Intermetallic Phase Observed upon Crystallization of La50Al25Ni25 Metallic Glass

The yet unknown intermetallic phase La₅Al₃Ni₂ was obtained by partially crystallizing amorphous La₅₀Al₂₅Ni₂₅ at 550 K (further heating above 600 K leads to irreversible disappearance of this phase), and its crystal structure was determined from X‐ray powder diffraction data. The crystal structure of the La₅Al₃Ni₂ phase constitutes a new structure type (Cmcm, a = 14.231Å, b = 6.914Å, c = 10.460Å, oC40) and is built from [Al₃Ni₂] chains surrounded by La atoms. In the ternary system La‐Al‐Ni La₅Al₃Ni₂ is located on the section La₅₀Al_50−nNi_n (0 ≤ n ≤ 50) with the binary compounds LaAl and LaNi as end members. Strikingly, also the crystal structures of the end members can be conceived as chain structures with Al and Ni chains surrounded by La, respectively.     

Mössbauer and X-ray diffraction characterization of Fe60Al40 coatings prepared by thermal spraying

Microstructured (atomized) and nanostructured (milled) Fe₆₀Al₄₀ powders together with their corresponding coatings synthesized by High Velocity Oxy-fuel (HVOF) or Atmospheric Plasma Spray (APS) thermal spraying techniques have been characterized by Mössbauer Spectroscopy (MS) and X-ray Diffraction (XRD). The evolution of the microstructure and the atomic ordering degree in the powders and coatings are discussed at the light of the various processing conditions. The operational correlation between the parameters of the duplex morphology of coatings and the processing parameters is discussed.