高纯氧化钇中镧、铈、钐、铝、铅和铜的电感耦合等离子体原子发射光谱法测定

本文以纯Y_2O_3中杂质元素的ICP-AES测定为例,研究用数值微分技术解决光谱干扰同题。结果表明,导数光谱法不仅可以有效地消除来自基体的光谱干扰,还能减小谱线干扰对检测能力的影响。当分析物浓度较低时,导数光谱法的加入回收率明显优于离峰分析法,多数情况下也优于在峰法校正光谱干扰时的回收率。     

Growth and Spectral Properties of Yb^3＋-doped Ba3Gd（BO3）3 Crystal

Crystal of Yb3+-doped Ba3Gd(BO3)3 has been grown by the Czochralski method. The spectroscopic characterizations have been investigated at room temperature. The Yb3+:Ba3Gd(BO3)3 crystal exhibits broad absorption at 976nm with FWHM of 7nm and large overall spitting of 2F7/2 manifold (823cm-1). The absorption and emission cross sections are 5.09×10-21cm2 at 976nm and 0.97×10-21cm2 at 1040nm,respectively. The fluorescence lifetime is 2.84 ms.     

稠杂环化合物的研究（XV）──6－取代－3－（1H－苯并三唑－1－亚甲基）－1，2，4－三唑并［3，4－b］－1，3，4－噻二唑的合成

研究了３－（１Ｈ－苯并三唑－１－亚甲基）－４－氨基－５－巯基－１，２，４－三唑与取代苯甲酸在三氯氧磷催化下的反应，制得１０种新的３－（１Ｈ－苯并三唑－１－亚甲基）－１，２，４．三唑并［３，４－ｂ］－１，３，４－噻二唑，通过元素分析、ＩＲ、￣１ＮＭＲ和ＭＳ确证了它们的结构并讨论了其波谱性质。     

Synthesis and structural characterization of cobalt(II) and zinc(II) complexes with 2-(indazol-1-yl)-2-thiazoline (TnInA). X-ray characterization of [CoCl2(TnInA)2] · C2H6O and [(M)(TnInA)2(H2O)2](NO3)2 (M = Co, Zn)

Several complexes of 2-(indazol-1-yl)-2-thiazoline (TnInA) with the divalent ions Co and Zn have been synthesized by the direct combination of the ligand and the metal chloride or nitrate hydrated salts in ethanol. These complexes have been characterized by a variety of physical–chemical techniques. Moreover, the structures of [CoCl₂(TnInA)₂] · C₂H₆O (1) and [(M)(TnInA)₂(H₂O)₂](NO₃)₂ (M = Co, 3; Zn, 4) were determined by single-crystal X-ray diffraction. In all the complexes, the ligand TnInA bonds to the metal ion through the indazole and thiazoline nitrogen atoms. In complex 1 the environment around the cobalt ion may be described as a distorted octahedron with two TnInA ligands and two chlorine ligands. Compounds 3 and 4 are isostructural with a distorted octahedral geometry around the metal center, being linked to two water molecules and two TnInA ligands. However, in complex [ZnCl₂(TnInA)] (2) the zinc atom is four-coordinated with a probable tetrahedral environment with two chloro ligands and one TnInA ligand bonded to the metal ion.     

Non-destructive and clean prediction of aviation fuel characteristics through Fourier transform-Raman spectroscopy and multivariate calibration

The combination of Fourier transform (FT)-Raman spectroscopy and partial least squares (PLS) regression is proposed to be used in off-line kerosene quality control. Here, six important physico-chemical properties have been studied: Abel flash point, initial boiling point (IBP), 10% of distilled sample, final boiling point (FBP), total percentage of aromatic compounds (% aromatics) and viscosity. The Raman spectra were obtained directly from standard 2 ml glass vials ( mm), using a Bruker RFS 100 FT-Raman spectrometer, equipped with a 1064 nm Nd:YAG laser and a Ge detector, in back-scattering mode and accumulating 25 scans (150 s acquisition time) with a laser power of 300 mW. All Raman spectra were unit normalized in order to avoid the influence of the laser power into the regression models. Different Raman shift spectral ranges have been evaluated, the 193.5-1688.1 cm⁻¹ region being the most satisfactory one. Corrected standard errors of prediction of 1.9, 2.3, 2.8 °C, 0.19 cSt and 0.7% were obtained for flash point, IBP, FBP, viscosity and % aromatics, respectively. The influences of the glass vials, sample positioning and laser power have been studied, as well.     

Preparation of polyaniline‐sulfate salt ­by emulsion and aqueous ­polymerization pathway without using ­protonic acid

Aniline was polymerized directly into polyaniline‐sulfate salt without using protonic acid in this work. Polyaniline‐sulfate salt was prepared by emulsion and aqueous polymerization pathways. The dopant i.e. sulfate ion in polyaniline‐sulfate salt was generated from ammonium persulfate which was used for oxidizing aniline. Ammonium persulfate acts both as oxidizing agent as well as protonating agent in the polymerization process of aniline to polyaniline salt. The efficiency of oxidizing and protonating power of ammonium persulfate is increased by the use of surfactant. The activity of ammonium persulfate is further increased by the use of sulfuric acid as protonic acid. It may be necessary to consider the effect of sulfate ion which is generated during the oxidation process of aniline in the chemical polymerization of aniline to polyaniline salt by ammonium persulfate either aqueous or emulsion polymerization pathway in the presence of protonic acid/functionalized protonic acid. Copyright © 2001 John Wiley & Sons, Ltd.     

Hyphenation of column liquid chromatography and Raman spectroscopy via a liquid-core waveguide: chemometrical elimination of spectral eluent background

In column liquid chromatography (LC) coupled to conventional Raman spectroscopy (RS) removal of the spectral background of the eluent is often demanding, because of the strong signals of the organic modifier. A new chemometrical method is proposed, called the eluent background subtraction (EBS) method, which can correct for small shape and intensity differences of the eluent spectra. The variations in the eluent spectra are modelled using principal component analysis (PCA). The PCA loading vectors are subsequently used for eluent background correction of the elution spectra of the analyte. The loading vectors are fitted under these spectra by an asymmetric least-squares method. This method was successfully applied under various experimental conditions and performed much better than conventional background correction methods. Analyte detectability was improved by (weighted) averaging of all elution spectra and smoothing via a p-spline function.     

电爆炸箔断路开关的理论和实验研究

 采用金属箔电爆炸过程的二维数值计算模型，对含电爆炸金属箔断路开关的电感储能脉冲功率调节系统进行了数值计算。以此为基础，研制出了一种低电感型的电爆炸箔断路开关，并以4μF/75kV脉冲电容器组作为初级能源，13Ω电阻作为负载进行实验研究。研究结果表明：在负载上可获得约250kV，脉宽大于400ns的脉冲电压。     

S-5N全固态重复频率脉冲发生器

 主要介绍S-5N的结构及测试实验结果。S-5N型全固态重复频率脉冲发生器是目前国际上同类源中峰值功率和平均功率均为最大的一台。随负载大小的变化，S-5N脉冲发生器的输出电压为400～600kV，输出电流2～3kA，输出脉冲半高宽40～50ns，单脉冲输出能量40～65J。 S-5N脉冲发生器在300Hz重复频率条件下可连续工作，500Hz重复频率条件下可连续工作3min，平均输出功率高达30kW。     

基于开关控制的兴趣实验设计

设计了开关控制实验,专门对常见的开关特点及使用进行探讨,根据开关特点搭建相应的控制电路,用近似于工程项目的形式锻炼学生对开关的灵活应用,激发了学生实验的兴趣和积极性.