Study of deposition offset in plasma spray of zirconia

Numerical modeling and experimental measurements have been performed to study the effects of powder carrier gas flow rates and powder sizes on the deposition offset in a plasma spray of yttria-stablized zirconia. The mathematical model involved simultaneous solution of the continuity, momentum and energy equations of the plasma gas, the dynamics and heat transfer of powder particles in the plasma, and the coupling effects between the plasma and panicles. Experiments included measurement of particle velocities by laser strobe technique and measurement of deposition offset. Calculated plasma temperatures and velocities are greater than 13,000 K and 2,000 m/s, respectively, in the vicinity of nozzle exit. For the plasma-particle momentum transfer, the drag coefficient was computed in two ways- with corrections accounting for the strongly varying plasma properties, and without these corrections. Calculated and experimental results, in respect to deposition offset, are in agreement to within 25% when calculated without varying properties corrections, and within about 40% with corrections; agreement in respect to average particle velocities is within 20% when calculated without varying properties corrections, and within the range 30–50% with corrections.     

Flow Injection Chemiluminescence for the Determination of Estriol via a Noncompetitive Enzyme Immunoassay

A novel approach to the detection of estriol using a flow injection system coupled to enhanced chemiluminescent immunoassay was developed based on noncompetitive immunoassay formats. A conjugated estriol-ovalbumin immobilized immunoaffinity column was inserted into the flow system to trap the unbound horseradish peroxidase (HRP)-labeled antibody after an off-line incubation of estriol and HRP-labeled anti-estriol antibody. The trapped enzyme conjugate was detected by the injection of chemiluminescent substrates to produce enhanced chemiluminescence. The linear range for the determination of estriol is 10.0 to 400 ng · mL⁻¹ with a correlation coefficient of 0.996 and a detection limit of 5.0 ng · mL⁻¹. The total time for sampling and chemiluminescent detection of one sample is 400 seconds after 30 min of pre-incubation. The results for pregnancy serum samples obtained by this method are in good agreement with those obtained using ELISA.     

Trace lead measurement and on-line removal of matrix interference in seawater by isotope dilution coupled with flow injection and ICP-MS

Isotope dilution analysis method coupled with flow injection and inductively coupled plasma mass spectrometry (ID-FI-ICP-MS), enabled trace lead concentration in seawater to be determined and the high salt concentration in the matrix, such as Na⁺, Ca²⁺ and Mg²⁺, to be removed on-line. The operational parameters of the FI system including pH for the chelating reaction, concentration of 8-hydroxyquinoline-5-sulfonic acid (8-HQS), sample loading time and injection speed, washing time and speed, eluting acid concentration and eluting speed, and instrumental parameters for ICP-MS were optimized and selected. Accurate results could be achieved because the isotope ratios required can be precisely measured in the range of the eluting peak by means of ID-FI-ICP-MS. The 3σ detection limit was 0.204 ng ml⁻¹. The trace lead concentration of seawater in south Xiamen, China was 0.988 ± 0.039 ng ml⁻¹. The recoveries of spiked Pb standard in seawater and standard reference water (GBW 08607) were 97.9 and 101.0%, respectively, with a relative standard deviation of 0.98%. This method can be used to determine trace lead concentration in high salt matrix samples, and is especially useful when the eluting peaks do not have a Gaussian-distribution.     

Preconcentration of trace elements from natural water with palladium precipitation

Palladium salts can be used as a coprecipitation carrier for the preconcentration of trace elements from natural water prior to their measurement by atomic spectrometry (AAS). The palladium is subsequently reduced by the introduction of hydrogen gas into the sample solution. The procedure is applied to the determination of Cu, Pb and Cd in seawater (enrichment factor 50) and synthetic water samples. Operating conditions have been optimized for the analysis of real samples. With the technique established an enrichment factor (500 fold) is feasible in synthetic samples. The recoveries of Cu, Cd and Pb from seawater are 95, 103 and 100%, respectively. This simple and rapid method can be applied in a wide pH-range and with complex matrices.     

Transition metal substituted tungstophosphoric compound catalyzed oxidation of hexanol to hexanal with hydrogen peroxide

Summary The oxidation of hexanol in the presence of the Keggin-type heteropoly compounds (HPCs) H₃PMo_nW_12-nO₄₀ (denoted as PMo_nW_12-n, n=0,1) and Na₅PW₁₁ZO₃₉ (denoted as PW₁₁Z, Z = Mn, Fe, Co, Ni, Cu and Zn) was carried out to produce hexanal and hexanoic acid. The reaction was conducted in tert-butanol (t-BuOH), using cetylpyridinium bromide (CPB) salts of HPA and 15% aqueous H₂O₂ as oxidant under mild condition. The PMoW₁₁ catalyst showed higher hexanol conversion of 25%, the lowest selectivity to hexanal of 64.4% and an efficient utilization of H₂O₂ of 34%. Over the transition metal substituted PW₁₁Z catalysts decomposition of H₂O₂ was rapid. For these PW₁₁Z catalysts, the efficient utilization of H₂O₂ decreased to 9% or even lower. By means of IR, UV-visible and GC-MS techniques the catalysts were characterized.     

(4,4′,4″,4″′-四硝基)·酞菁合钴(Ⅱ)化学修饰电极对抗坏血酸的电催化氧化

合成了一种钴的酞菁配合物,以玻碳为基体、用化学吸附法制备了它的化学修饰电极。用CV法研究了该化学修饰电极对抗坏血酸氧化的电催化作用。结果表明,该化学修饰电极对抗坏血酸的氧化有一定的电催化作用,且电催化活性的稳定性高,抗坏血酸的电催化氧化峰电流和其浓度之间有良好的线性关系。     

分子的模糊对称性

将模糊数学方法引入对分子对称点群的研究,建立描述具有不完整分子对称性的模糊点对称群(集合).建立具有模糊对称性分子轨道的模糊表示及其模糊特征标(模糊广义宇称).通过对典型的线状分子、平面分子以及非平面的立体分子等进行分析,展示了一个新的理论化学园地.初步探讨了具有模糊对称性的动态反应体系.从模糊对称性出发,探讨了分子轨道对称守恒原理的半定量特征.     

苯乙烯基氮氧杂芳烃间的交叉光二聚反应

用中压汞灯(λ > 300 nm)照射4-苯乙烯基吡啶、2-苯乙烯基苯并噁唑和5-苯基-2-苯乙烯基噁唑三种杂芳基乙烯单体中任意两种的硫酸水溶液，得到三种交叉二聚体.用高效液相色谱跟踪研究了交叉光二聚反应，发现每组反应生成三种光二聚体，其中二种为单体自身的光二聚体，而另外一种是两种不同单体的交叉光二聚体.交叉二聚体通过柱色谱分离得到，其顺式头对尾结构经紫外、红外、氢谱、碳谱和元素分析确定.用紫外光谱和高效液相色谱跟踪研究了交叉光二聚体的稀溶液在低压汞灯（λmax=254 nm）照射下的光解反应.研究发现交叉二聚体能够彻底发生光解，首先生成原来的反式单体，所生成的反式单体容易发生异构化而生成顺式单体，最终建立起反顺异构化平衡.     

FIA-ICP/AES法分析茶叶浸取液中多元素的形态

本文报道了分析茶叶浸取液中[Zn、Mn、Fe、Al及Mg]形态的新方法。研究了以C-18柱为分离柱的流动注射与ICP/AES的联用技术。     

CAHN－2000磁天平的调试与数据处理系统的研制

叙述了ＣＡＨＮ－２０００磁天平（美国）调试过程中如何解决液氮温区的测试，自制了磁天平与计算机的接口，编写了数据采集、处理和控制等高原 软件，节省了几万美元，部分指标超过原配套水平，三年来仪器在对国同外开放过程中，液氮温区的工作一直正常，实测了上千个样品，提供的数据已撰写数十篇文章在国内外刊物上发表。由此说明，要充分发挥进口仪器的使用效率，必须对仪器的工作原理、结构特点有透乇的了解，同时要有相当的自