化学衍生-高效液相色谱法测定硫氰酸根阴离子

以α-溴-2,3,4,5,6-五氟甲苯作柱前衍生试剂,经优化衍生和色谱条件,实现了用高效液相色谱法测定硫氰酸根离子。在ODS柱上,用甲醇-水(80:20)作流动相,于254nm检测,得到线性关系良好的工作曲线,最小检测限为4.7ng。分析了吸烟者唾液样品,回收率为93.7％～101.4％。     

用非等温TG、DTG曲线研究由邻香兰素衍生的Cu(Ⅱ)希夫碱配合物的热分解反应动力学

研究表明,许多过渡金属配合物具有抗癌抑菌性能,刃我们在以前工作基础上又合成了三种由邻香兰素衍生的新型希夫碱配合物,对他们进行了非等温热重分析,并采用积分法和微分法相结合的方法,推断出了它们的热分解反应机理.     

氢化物发生石墨炉原位富集直接测定高温镍基合金中碲

通过选择碲的氢化物发生条件，克服了高含量镍对碲的干扰，把氢化物富集在涂钯石墨管里，然后再原子化，成功地测定了高温镍基合金中碲。     

丙烯酸三苯基锡酯及其聚合物的合成和表征

合成了丙烯酸三苯基锡酯及其聚合物，通过ＩＲ、￣１ＨＮＭＲ、￣（１３）ＣＮＭＲ对其结构进行了表征，推断单体中的锡原子与羰基氧原子间存在分子间的配键，锡原子的配位数是５，而聚合物没有形成锡氧配键。     

一阶导数光谱K系数法同时测定硝基酚钠三组分

研究和建立了同时测定硝基酚钠混合三组份的新方法——一阶导数光谱K系数法。确定了最佳实验条件和测定波长,方法简便、快速、准确。通过对动植物细胞赋活增进剂中邻硝基酚钠、对硝基酚钠、5-硝基愈创木酚钠三组份的直接测定,其相对误差小于2%,相对标准偏差小于3%,回收率为99～103%。     

Chemiluminescence flow system for the determination of ammonium ion

A novel chemiluminescence (CL) system for ammonium ion combined with flow-injection analysis is presented in this paper. It is based on the CL reaction between luminol, immobilized electrostatically on an anion-exchange column, and chlorine electrochemically generated on-line via a platinum electrode from hydrochloric acid in a coulometric cell. Ammonium ion reacts with chlorine and decreases the observed CL intensity. The system responds linearly to ammonium ion concentration in the range 1.0-100 muM, and the detection limit is 0.4 muM. A complete analysis, including sampling and washing, could be performed in 1 min with a relative standard deviation of <6.0%. The system is stable for over 500 determinations and has been applied successfully to the determination of ammonium ion in rainwater samples.     

Synthesis and characterization of highly ordered mesoporous thin films with -COOH terminated pore surfaces

Highly ordered mesoporous inorganic-organic hybrid thin films with covalently bonded carboxylic acid (-COOH) terminal groups on the pore surfaces were synthesized by evaporation induced self-assembly of tetraethoxysilane, organosilanes, and a nonionic surfactant followed by acid hydrolysis and characterized using transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, surface acoustic wave (SAW) based N2 sorption, and thermogravimetric analysis (TGA) techniques.     

STRUCTRE AND PROPERTIES OF COMPOSITE Ni/HARD CARBON FILMS PREPARED BY PLASMA DEPOSITION

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Molecular recognition and conductance in crown ethers

Crown ethers have the remarkable property of recognizing and binding specific metal cations in complex mixtures. We propose to combine molecular recognition with molecular electric conductance. The question we address is: can the event of binding a cation be sensed by a change in conductance? Specifically, we study a short molecular wire (MW) containing a crown-6 molecule connected via sulfur atoms to two gold atomic wires acting as metallic leads. Upon binding a cation, the density of states of the system is only slightly affected. This reflects the fact that the cation binding is largely electrostatic in nature and is accompanied by little electronic reorganization. Yet, the cationic binding does significantly lower conductance. We also identify strong interference affecting the conductance. A striking feature is the insensitivity of conductance to the type of ligand with the exception of the proton.     

A study of thoria on the surface of gamma-Al2O3

The dispersion of thoria on the surface of gamma-Al2O3 and the surface properties of ThO2/gamma-Al2O3 samples, as well as the influence of the loading amount of thoria on the reduction behavior of copper oxide species, have been studied using XRD, XPS, FTIR, and TPR. The results indicate that the dispersion capacity of thoria, like that of ceria, is much lower than for two other tetravalent metal oxides, zirconia and titania, and the surface adsorption amount of the carbonyl compound and H2O slightly increases with increasing thoria loading. The different thoria loadings can influence the reduction behavior of the dispersed copper oxide by comparing the TPR results of CuO/ThO2/gamma-Al2O3 samples. In addition, the lower dispersion capacities of thoria and ceria on gamma-Al2O3 are tentatively discussed by considering the structural stability of the two oxides.