High-performance liquid chromatography of some basic drugs on a n-octadecylphosphonic acid modified magnesia-zirconia stationary phase

The high-performance liquid chromatographic behavior of some basic drugs was studied on a n-octadecylphosphonic acid modified magnesia-zirconia (C18PZM) stationary phase. The effect of mobile phase variables such as methanol content, ionic strength, and pH on their chromatographic behavior was investigated. The retention mechanism of basic drugs on the stationary phase was elucidated. The results indicate that both hydrophobic and cation-exchange interactions contribute to solute retention under most chromatographic conditions. The inherent Br?nsted-acid sites and also the adsorbed Lewis base anionic buffer constituents on accessible ZM surface Lewis acid sites play a role in the retention of ionized solutes by cation-exchange interaction. However, especially at high mobile phase pH, the retention of basic drugs depends mainly on hydrophobic interactions between solutes and support. Separations of the basic drugs on the C18PZM phase by a predominantly reversed-phase retention mode were very promising. The mixed-mode retention feature on this phase, as a result of the adsorbed Lewis base anionic buffer constituents acting as sites for cation-exchange, could also be very useful, e.g. for enhancing the chromatographic selectivity of such analytes. The C18PZM seems to be an excellent alternative to silica-based reversed-phase stationary phase for the separation of strongly basic solutes.     

飞秒激光脉冲作用下氧化镁的烧蚀及其超快动力学过程

研究了双面抛光氧化镁单晶（111）表面800 nm飞秒激光单脉冲烧蚀阈值和激光脉宽的依赖关系.利用泵浦-探针技术,测量不同能量和脉宽作用下飞秒激光烧蚀的时间分辨反射率的演化.通过扫描电镜观察其烧蚀形貌,发现大量的沿氧化镁［100］晶向开裂的裂纹.讨论了表面裂纹的形成机理,并解释了飞秒激光烧蚀氧化镁的超快动力学过程.     

V2O5/MO-Al2O3（M = Mg，Ca，Sr，Ba）催化剂用于正丁烷催化氧化脱氢反应

采用浸渍法制备了不同V2O5担载量的V2O5/MO-Al2O3(M = Mg, Ca, Sr, Ba)催化剂,钒物种的前驱体为偏钒酸铵.对制备的催化剂进行了一系列表征,并对催化剂上正丁烷选择性氧化脱氢制取丁烯进行了反应研究.表征结果(包括比表面积、X射线衍射、傅里叶红外光谱、氢气程序升温还原和拉曼光谱)显示,不同碱土金属元素掺杂的催化剂显示不同的钒价态信息和催化性能.其中掺杂Ca, Sr, Ba的催化剂,正钒酸盐相很难被还原,因此催化剂的氧化还原循环难以建立,导致以上三种催化剂在正丁烷氧化脱氢反应中活性较低.然而, Mg掺杂的催化剂却显示出较高的催化活性和选择性.实验结果表明：在Mg掺杂的载体上担载5% V2O5的催化剂上600°C时可获得高达30.3%的正丁烷转化率和64.3%的烯烃总选择性.这与V2O5担载量为5%时,在获得高度分散的钒氧化合物物种时可使MgO晶相稳定存在密切相关.     

添加Li+对MgO催化性能的影响

本文以IR、TPD、丁烯异构化及直接脱氢反应为手段,对不同Li⁺添加量的MgO催化剂进行了研究。结果表明,表面低配位氧集团是催化剂的主要活性物种,起碱中心作用;表面金属离子起L酸中心作用。酸、碱中心的数目、强度随Li⁺添加量不同而呈规律性变化。这种变化影响了酸、碱中心的协同作用,从而影响其催化活性。     

Positron annihilation and electrical studies on the influence of loading magnesia nanoribbons on PVA-PVP blend

This work aims to study the effect of loading magnesia (0.5–2.0 wt%) on the positron annihilation parameters and electrical properties of the PVA-PVP blend. The films were synthesized by solution casting and checked by different techniques. XRD and HR-TEM of sol-gel prepared magnesia revealed that the average crystallite size was 14.29 nm with ribbon-like morphology with varying widths and lengths up to a few micrometers. SEM showed that the blend surface appeared smooth and homogenous and this confirmed the compatibility between PVA and PVP. However, loading magnesia increased surface roughness. TGA confirmed the thermal stability enhancement of blend film with magnesia incorporation. Ortho–positronium lifetime τ₃ and the free volume $V_f$ decrease with loading magnesia while the intensity I₃ is nearly constant. These features were interpreted in view of the hole-filling mechanism, the interaction between magnesia & blend and magnesia morphology. The equilibrium swelling ratio ESR was found for the studied films and a positive correlation between ESR and $V_f$ was reported. The current density-electric field, J-E, characteristics were of non-ohmic type. J increased with increasing magnesia levels and heating. The Richardson-Schottky effect was the dominant dc conduction mechanism at low temperature and low magnesia loading levels while it changed to Poole–Frenkel emission at higher values. Finally, a correlation between Log J and the intensity I₂ was reported.     

Surface resistance measurements at the metal/electrolyte interface of Ag(100) and Ag(111) thin film electrodes

The conductivity of thin film metal electrodes with a thickness of the order of the mean free path of the conduction electrons (50 nm at 300 K) is sensitive to several processes on the metal surface (e.g. adsorption and desorption of ions). We developed epitaxially grown Ag(100)/MgO(100) and Ag(111)/TiO₂(110) electrodes of 20 nm thickness. The change in the surface resistance of Ag(100) thin film electrodes during adsorption of the halide ions Cl⁻, Br⁻ and I⁻ shows the different strengths of specific adsorption. We investigated the phase transition of thiocyanate (SCN⁻) on Ag(100) electrodes by combining the surface resistance method with voltammetric, capacitance and ex-situ XPS measurements. The influence of adsorbed uracil on the resistance of Ag(100) films was demonstrated. The surface resistance is very sensitive to small concentrations of metal cations (e.g. Tl⁺). The surface resistance of Ag(100) and Ag(111) thin film electrodes shows the typical difference in the stripping potential of Tl⁺ of about 100 mV.     

菱面片层氧化镁的制备及晶格畸变与反常红外特性

以低品位白云石为原料采用二次酸浸、EDTA-氨水沉淀法制备前驱体Mg（OH）2，经煅烧得到菱面片层状多空隙结构的纳米MgO晶体。通过X射线衍射（XRD）、高分辨率扫描电镜（HRSEM）及傅立叶红外光谱（FT—IR）等测试手段对所得产物的物相和形貌等进行了表征。分析表明：氧化镁为结晶良好、立方晶系，厚度约10～20nm，最大面积可达1μm^2左右的菱形纳米片层结构；XRD数据表明纳米氧化镁的微结构存在晶格畸变并导致XRD相位差发生变化；红外光谱表明，Mg-O键伸缩特征吸收峰向高波数方向移动（蓝移）了约84．82cm^-1，而弯曲特征吸收峰向低波数方向移动（红移）了约31．88cm^-1，并导致红外吸收光谱的宽频化。结合XRD数据分析结果和界面效应等物理现象讨论了反常红外吸收机理。     

Studies on the Catalytic Properties of Magnesia Supported on γ-Alumina

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FAAS法同时测定工业氧化镁中杂质元素钙,铁,锰的研究和应用

本文就火焰原子吸收法测定工业氧化镁中杂质元素钙，铁和锰的条件进行了试验，对基体元素的影响和消除方法进行了探索。所建立的方法应用于工业氧化镁产品中的铁，钙和锰的分析，结果与国家标准方法分析结果相比较，经统计检验，两者无显著性差异。相对标准偏差钙为１．４１％，铁为３．２０％，锰为０．９６％。方法简便，快速，准确，可用于工业氧化镁产品的质量检验。     

Influence of magnesia modification on the properties of copper oxide supported on gamma-alumina

XRD, BET, TPR, UV-vis DRS and in situ FT-IR were employed to investigate the dispersion, reduction and CO(2)-adsorption behaviors of copper oxide supported on magnesia modified gamma-Al(2)O(3) (Mg-Al) samples. The results indicate that magnesia could be highly dispersed on the surface of gamma-Al(2)O(3) to form a monolayer and the dispersion capacity is about 1.55 mmol/(100 m(2)gamma-Al(2)O(3)). For copper oxide supported on Mg-Al samples, both the dispersion capacity and the reduction temperature of surface CuO decrease with the MgO loading. CO(2)-adsorption IR results show that the surface strong basic amount for the catalysts increases with the dispersed MgO loading. In addition, the activity of CO oxidation suggests that the main active species in this system should be small CuO cluster and the existence of dispersed MgO enhances the activity of CO oxidation. The catalysts might be applied in pollution control devices for vehicle exhaust, CO gas sensors, catalytic combustion and gas purification of CO(2) lasers. All the results have been discussed by the consideration of the variation of gamma-Al(2)O(3) surface structure before and after magnesia modification.