红外吸收法测定碳化铪粉末中的氧含量

应用氧氮分析仪建立碳化铪粉末中氧的测定方法。针对碳化铪熔点极高的特性,对加热功率、称样量和空白值等测定条件进行探讨,选择适合的助熔剂和高温石墨坩埚,确定了最佳测试条件。将该方法用于实际样品测定,测定结果的相对标准偏差小于2.0%(n=9),样品的加标回收率为98.1%～102.6%。     

Influence of the anode material on the characteristics of an analytical glow discharge cell

The energy transfer to the discharge gas due to various collision processes in the plasma and the heating of the sample are widely known effects in glow discharge (GD) spectroscopy. Despite of the considerable thermal effects and their serious influence on the performance of GD devices, measurements of the discharge gas and sample temperatures are not common at all. The gas temperature depends on the power absorption of the discharge as well as on the temperature of boundaries (sample and anode). In this work the influence of different anode materials in a Grimm-type source on the voltage–current characteristics, crater shapes and GD spectra is investigated. Anodes made of titanium and copper alloys, graphite, and steel with thermal conductivities covering a wide range of values are used. For a fixed voltage and pressure a decrease of the measured current is observed for bad thermal conductive anodes. Cooling of the sample results in an increase of the measured current. Both observations can be explained by changes of the discharge gas temperature. The temperature of the sample is measured from the back side and compared for different anodes. Further, it is found that the choice of the anode material (i) has no significant influence on the crater shape, (ii) results in slightly different sputtering rates and (iii) strong differences of the GD spectra.     

Fast oxidation of secondary alcohols by the bromate-bromide system using cyclic microwave heating in acidic water

We report an improved, gentle, cyclic microwave activation technique for the oxidation of secondary alcohols using nonhazardous hypobromous acid (BrOH) as the reagent in acidic water. Several aliphatic and aromatic secondary alcohols were successfully oxidized to the corresponding ketones using this technique in high yields and with only minor amounts of side products.     

Preparation of magnetic indole-3-acetic acid imprinted polymer beads with 4-vinylpyridine and β-cyclodextrin as binary monomer via microwave heating initiated polymerization and their application to trace analysis of auxins in plant tissues

Auxin is a crucial phytohormone for precise control of growth and development of plants. Due to its low concentration in plant tissues which are rich in interfering substances, the accurate determination of auxins remains a challenge. In this paper, a new strategy for isolation and enrichment of auxins from plant tissues was obtained by the magnetic molecularly imprinted polymer (mag-MIP) beads, which were prepared by microwave heating initiated suspension polymerization using indole-3-acetic acid (IAA) as template. In order to obtain higher selective recognition cavities, an enhanced imprinting method based on binary functional monomers, 4-vinylpyridine (4-VP) and β-cyclodextrin (β-CD), was adopted for IAA imprinting. The morphological and magnetic characteristics of the mag-MIP beads were characterized by scanning electron microscopy, Fourier-transform infrared spectroscopy and vibrating sample magnetometry. A majority of resultant beads were within the size range of 80-150μm. Porous surface morphology and good magnetic property were observed. Furthermore, the mag-MIP beads fabricated with 4-VP and β-CD as binary functional monomers exhibited improved recognition ability to IAA, as compared with the mag-MIP beads prepared with the individual monomer separately. Competitive rebinding experiment results revealed that the mag-MIP beads exhibited a higher specific recognition for the template than the non-imprinted polymer (mag-NIP) beads. An extraction method by mag-MIP beads coupled with high performance liquid chromatography (HPLC) was developed for determination of IAA and indole-3-butyric acid (IBA) in plant tissues. Linear ranges for IAA and IBA were in the range of 7.00-100.0μgL(-1) and 10.0-100.0μgL(-1), and the detection limits were 3.9 and 7.4μgL(-1), respectively. The analytical performance was also estimated by seedlings or immature embryos samples from three different plant tissues, pea, rice and wheat. Recoveries were in the range of 70.1-93.5%. The results show that the present imprinting method is a promising approach for preparation of selective adsorbents for sample preparation of auxin analysis in plant tissues.     

Ion Heating in Dusty Plasma of Noble Gas Mixtures

Ion heating in dusty plasma of noble gas mixtures is studied by the observation of dust particles in stratified glow discharge. The particles and their formations can be used as a “contact‐free” probe of the ion flows. It is shown that under condition of experiments transition of dust particles into crystalline state in pure gases occur at much lower pressures in comparison to the case of gas mixtures. This observation is also supported by the evaluation of “effective” kinetic temperature of dust particles as defined from the velocity distribution function at the same set of discharge parameters. Absolute value of temperature of dust component in the mixture of helium and argon indicates important role of argon ionization process (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Grafting of bifunctional phosphonic and carboxylic acids on Phynox: Impact of induction heating

Phynox, a cobalt-chromium alloy, exhibits interesting mechanical properties making it a valuable material for a number of applications. However, its applications (especially biomedical ones) often require specific surface properties that can be imparted via suitable surface functionalizations. Based on Faraday's law of induction, induction heating is a widely used method to heat metallic substrates directly and contactless. The aim of this work is to compare the influence of induction heating and a conventional heating method on the functionalization of Phynox surfaces with bifunctional (6-phosphonohexanoic and 11-phosphoundecanoic acids) monolayers in order to create a platform for a large variety of post-grafting chemical reactions, e.g. with alcohols and amines, to modify and control the surface properties. In a first part, we assess the influence of the heating method on the interaction between the two terminal moieties of the 6-phosphonohexanoic and 11-phosphoundecanoic acids and the Phynox surface by studying the grafting of n-dodecylphosphonic acid and n-dodecanoic acid separately. The suitability of such bifunctional molecules for post-grafting chemical reactions has then been assessed by studying the post-grafting of a fluorinated alcohol by the Steglich esterification reaction between the carboxylic end of the grafted bifunctional molecules and the alcohol function of the post-grafted molecule. It has been shown that induction heating can lead to a much more selective adsorption of bifunctional molecules on the surface of Phynox, leaving a higher amount of free carboxylic acid functions to react during the second modification step.     

Excimer laser accelerated hydrothermal synthesis of ZnO nanocrystals & their electrical properties

The synthesis of ZnO nanocrystals is reported using a hydrothermal chemical growth technique combined with 248 nm nanosecond excimer laser heating at fluences in the range 0-390 mJ cm⁻². The effect of laser heating in controlling the morphology of the nanocrystals is investigated using optical spectroscopy and electron microscopy characterization. Laser heating is shown to allow control of the crystal morphology from nanoparticles to nanorods as well as to modify the size distributions. The results indicate that not only does the laser accelerate the growth of nanocrystals, but can also produce crystals with a narrow size distribution possibly via photothermal size selection. An initial study of electrical conduction properties of ZnO nanocrystal thin films is also discussed.     

高温及超高温热管的启动特性和传热极限

根据局部高温、高热流加热等特殊场合的需求,设计、加工了钠高温热管及锂超高温热管,并对热管的启动和极限特性进行了研究。高温及超高温热管能够顺利启动,但启动时应注意可能到来的声速传热极限。端部加热启动时,端部附近管体部分会形成一段等效的加热段,可以将工质从启动时的固体状态到全部熔化形成相变传热及流动循环的时间确定为启动时间。热管的传热极限特性表明,超高温热管应工作在更高的温度和更大的热流密度。热管的结构和工艺优化有利于启动和运行。     

端部周期加热下管内气温奇异分布的实验研究

设计搭建了端部周期加热时管内气体热声对流的实验平台,对端部周期加热引起的气体热声对流作用下管内气体的温度分布进行了实验研究。该实验以氩气为工质,利用三极管控制加热电路实现周期性加热;测量了不同加热频率下管内的气体温度,并与常热流加热时的温度分布进行对比,结果表明端部周期加热时管内气体的温度分布与同功率下常热流加热时存在明显的差异,并且在某些测点出现了温度的奇异分布。本实验验证了超温现象的存在,为管内气体热声对流现象的进一步研究奠定了基础。     

Hybrid resonance of Maxwell's equations in slab geometry

Hybrid resonance is a physical mechanism for the heating of a magnetic plasma. In our context hybrid resonance is a solution of the time harmonic Maxwell's equations with smooth coefficients, where the dielectric tensor is a non-diagonal Hermitian matrix. The main part of this work is dedicated to the construction and analysis of a mathematical solution of the hybrid resonance with the limit absorption principle. We prove that the limit solution is singular: it consists of a Dirac mass at the origin plus a principal value and a smooth square integrable function. The formula obtained for the plasma heating is directly related to the singularity.