横向和纵向加热涂钨平台石墨炉原子吸收光谱法测定镓的比较

分别优化了横向加热和纵向加热涂钨平台石墨炉原子吸收光谱法测定镓的条件。结果显示,纵向加热方式的原子化温度比横向加热低,在灰化温度、进样量、酸介质的影响和化学改进剂等方面,两者没有显著差别。纵向加热的灵敏度高于横向加热,线性范围也比横向加热宽;但是采用横向加热方式能获得更低的检出限和更强的抗干扰能力。     

Highly sensitive detection of silybin based on adsorptive stripping analysis at single-sided heated screen-printed carbon electrodes modified with multi-walled carbon nanotubes with direct current heating

A new disposable multi-walled carbon nanotubes modified single-sided heated screen-printed carbon electrode (MWNT/ss-HSPCE) was fabricated. The electrochemical behavior of silybin was investigated by cyclic voltammetry and the probable electrode reaction mechanism was proposed. A simple and cheap direct current heating supplier was used to heating the electrode for adsorptive accumulation of silybin. The square wave voltammetric stripping peak current of silybin at MWNT/ss-HSPCE with an elevated electrode temperature of 50 °C only during accumulation step was dramatically improved compared with that at bare single-sided heated screen-printed carbon electrode (ss-HSPCE) without heating. This enhancement was mainly contributed to the combination of the advantages of multi-walled carbon nanotubes and electrically heated electrodes. Under optimum conditions, two detection linear ranges of silybin were from 1.0 × 10⁻⁹ to 1.0 × 10⁻⁷ M and 3.0 × 10⁻⁷ to 1.0 × 10⁻⁶ M. A detection limit of 5.0 × 10⁻¹⁰ M could be obtained (S/N = 3), which was more than two magnitudes lower than that at bare ss-HSPCE without heating. To the best of our knowledge, this was also at least two magnitudes lower than any others for electrochemical detection of silybin in the literature. Finally, the method was successfully applied to the determination of silybin in pharmaceutical tablets.     

Second law analysis of water flow through smooth microtubes under adiabatic conditions

In the study, a second law analysis for a steady-laminar flow of water in adiabatic microtubes has been conducted. Smooth microtubes with the diameters between 50 and 150 μm made of fused silica were used in the experiments. Considerable temperature rises due to viscous dissipation and relatively high pressure losses of flow were observed in experiments. To identify irreversibility of flow, rate of entropy generation from the experiments have been determined in the laminar flow range of Re = 20-2200. The second law of thermodynamics was applied to predict the entropy generation. The results of model taken from the literature, proposed to predict the temperature rise caused by viscous heating, correspond well with the experimental data. The second law analysis results showed that the flow characteristics in the smooth microtubes distinguish substantially from the conventional theory for flow in the larger tubes with respect to viscous heating/dissipation (temperature rise of flow) total entropy generation rate and lost work.     

An internally heated composite gasket for diamond-anvil cells using the pressure-chamber wall as the heating element

The implementation of a heating element to a composite gasket for high-temperature applications in the diamond-anvil cell was developed based on a double-gasket assemblage. The heating element is a thin platinum wall that covers the central borehole of the metal–ceramic–metal composite gasket and interconnects the two metal component parts of the gasket. Applying electric powers up to 35 W to the two gasket metal components result in ring-like heating around the sample inside the pressure chamber with temperatures exceeding ～2000 K in individual cases. The ring-like distribution of the maximum temperature located at the pressure-chamber wall facilitates a homogeneous temperature distribution at the sample position. As a consequence of the concentration of the heating power to the pressure chamber region, gradients of surface temperatures, both at the gasket and the diamond anvil, appear to be more pronounced compared with those known for classical external electrical heating. Apart from the tests of the mechanical stability on high-pressure operation in the diamond anvil cell at room temperature, the influence of the anvils in contact with the gasket on the characteristic power–temperature curves, temperature gradients and thermal equilibration resulting from changes in electrical power settings have been evaluated within the scope of a series of experimental investigations.     

On-line laser heating setup for ED-XAS at ID24: preliminary optical design and test results

Double-sided laser heating (LH) combined with synchrotron X-ray radiation for in situ studies in the diamond anvil cell (DAC) has been the most productive and widely used high-temperature–high pressure technique in the past two decades. In the framework of the UPBL11 project (upgrade of ID24 beamline of European Synchrotron Radiation Facility), we developed a new on-line LH system for DACs. The preliminary optical scheme of the system is presented and discussed. Varying the settings, we are able to shape and to size the beam on the surface of the sample in the DAC. First pilot applications to the Fe case are shown.     

Single-crystal X-ray diffraction at megabar pressures and temperatures of thousands of degrees

The most reliable information about crystal structures and their response to changes in pressure and temperature is obtained from single-crystal diffraction experiments. We have developed a methodology to perform single-crystal X-ray diffraction experiments in laser-heated diamond anvil cells and demonstrate that structural refinements and accurate measurements of the thermal equation of state of metals, oxides and silicates from single-crystal intensity data are possible in pressures ranging up to megabars and temperatures of thousands of degrees. A new methodology was applied to solve the in situ high pressure, high temperature structure of iron oxide and study structural variations of iron and aluminum bearing silicate perovskite at conditions of the Earth's lower mantle.     

Industrial application of impulsive high pressures in sheet forming with parameter optimization

Abstract

Impulsive high pressures for sheet forming are widely used in the modem industry. Applied aspects of the impulsive forming problem, including both control external stress and heat influence parameters are stated in the present research. The problem is reproduced in the vector representation in the multidimensional space of optimizing functions. In the case of a limited number of measurements the task leads to well known scalar representations with similar physical characteristics'.     

High temperature diamond anvil cell with the laser heating

Abstract

Focusing laser radiation in the center of a diamond anvil cell (DAC) allows investigations up to P?100 GPa with the pulsed' and sustained heating to 5000 K^2,3. The use of laser radiation permits the exclusion of a heater if the sample itself strongly absorbs the radiation. Many materials are transparent for 1.06 μm YAG-laser radiation usually used for the heating. Therefore it is necessary to mix absorbing radiation powders, for example, graphite, platinum²³. The use of the powerful C0₂-laser for the heating considerably extends the scope of the materials under investigation, as the wavelength radiation Λ= 10 μm is in the range of the strong lattice absorption (absorption coefficient～ 10³-10⁴ cm-^l) of many oxides, nitrides and so on.     

长脉冲等离子体放电下HT-7装置限制器温度变化及能流分析

在HT-7托卡马克等离子体长脉冲放电过程中,作为直接面对等离子体的第一壁限制器表面的温度变化及其承受的能流密度的计算,对于判断限制器的作用和对等离子体的影响都有非常重要的意义。主要从测量到的距离限制器表面3mm处温度变化曲线,采用无限大平面模型计算限制器模头表面能量沉积的能流密度,并讨论了不同等离子体放电下局部点能流密度的差别。多数长脉冲放电下,少数局部点的温升超过1 000℃,最大能流密度超过10MW/m2;但通过对等离子体位移的控制,局部点温升被抑制,高密度能流持续时间短,有利于长脉冲放电。同时对限制器结构和材料对模头温度的影响也做了比较详细的分析。