Ln(Ⅲ)与2-羟基-1-萘醛缩蛋氨酸盐及邻菲咯啉三元配合物的合成与表征

合成了稀土硝酸盐与希夫碱盐2-羟基-1-萘醛缩蛋氨酸钾(以KL表示)及邻菲咯啉(Phen)的四种固体三元配合物。通过元素分析，IR，UV，DTA-TG及摩尔电导分析等手段确定配合物的组成为[Ln(L)(Phen)(NO3)(H2O)]NO3(Ln＝Gd，Dy，Er，Yb)，并对它们的配合方式及某些物理和化学性质进行了研究。     

Spectroscopy and Structure of Sol-Gel Systems

Sol-gel derived glasses may differ from conventional melt-quenched glasses owing to the peculiar microstructures existing at the gel state, such that, even after gel densification, some differences may remain in their composition and molecular structure.This paper discusses structural characteristics of thin film oxide gels and glasses, with a special emphasis on SiO2-TiO2 based systems, which are of particular interest for sol-gel integrated optics applications. Short range structure aspects are discussed based on infrared, X-ray photoemission and X-ray photoabsorption spectroscopies. The chemical homogeneity of sol-gel materials is evaluated, based on X-ray photoemission and nuclear magnetic resonance spectroscopies, dealing in particular with the issue of homo- vs. heterocondensation. Finally, some microstructural features of sol-gel derived films are analyzed, namely the relationship between infrared absorption and porosity and the structure of nanocrystalline sol-gel films, based on grazing incidence X-ray diffraction and micro-Raman spectroscopy. The types of structural information obtainable by each different technique are compared in detail.     

蒙脱土表面键合配位体固相萃取填料的制备及其对重金属离子的吸附性能

通过酸洗、硅烷偶联剂表面活化、键合苯甲酰异硫氰酸酯对蒙脱土进行改性,制得新型固相萃取(SPE)材料。 采用红外光谱、扫描电子显微镜、X射线光电子能谱表征了改性蒙脱土的结构和形貌。 考察了制备的SPE填料对水中As³⁺、Bi³⁺、Cu²⁺、Sb³⁺、Sn²⁺和Pb²⁺的吸附性能,确定了最佳固相萃取条件,对6种金属离子吸附容量分别为10.83、11.92、12.67、10.43、10.01及10.54 mg/g。 通过SPE与电感耦合等离子体质谱联用测定了样品中As³⁺、Bi³⁺、Cu²⁺、Sb³⁺、Sn²⁺和Pb²⁺ 6种重金属离子的含量,检出限分别为0.024、0.013、0.075、0.037、0.011和0.064 μg/L。     

聚[碳酸(亚丁酯-co-ε-己内酯)酯]的制备及其载药微球性能的研究

采用阴离子配位聚合方法, 合成了二氧化碳、1,2-环氧丁烷与ε-己内酯的三元共聚物: 聚[碳酸(亚丁酯-co-ε-己内酯)酯](PBCL). 并采用复相乳液(W/O/W)溶剂挥发法制备了包裹抗菌药物甲磺酸帕珠沙星的可降解微球. 对聚合物进行了FTIR, ¹H NMR, ¹³C NMR, DSC, TGA和WAXD等表征, 以及降解性能和载药微球特性的研究. 结果表明, PBCL热稳定性及降解性能优于聚碳酸亚丁酯(PBC). 所得PBCL微球球形规整、表面光滑. 大部分微球粒径在0.5～1 μm的范围内, 载药量和包封率分别达到38.21%和87.9%. 微球的体外释药性能研究在pH 7.4的磷酸缓冲溶液中进行, 释放21 d后, PBCL微球的累积释药量为84.74%, PBC微球的释药量仅为17.29%. 药物的体外释放行为符合Higuchi方程. PBCL载药微球具有长效缓释作用.     

离子液体相转移催化环己醇氧化制备环己酮

以不同种类的离子液体作为相转移催化剂,用双氧水作为氧化剂,Na2WO4·2H2O为催化剂,在适当的反应条件下,能有效进行相转移催化环己醇氧化制备环己酮.实验结果表明,采用酸性离子液体[C16mim]HSO4和[C14mim]HSO4相转移催化合成环己酮,可提高环己酮的产率,具有反应条件温和、操作简便、需用时间短、相转移催化剂可以循环使用等优点.在反应温度为90℃,反应时间为50min条件下,环己醇的转化率高达100%,选择性99%以上.     

微波等离子体炬发射光谱法去溶系统性能的研究

用微波等离子体矩（MPT）作激发光源，等离子体的工作气体为氩气，研究了气动雾化进样去溶系统的工作参数对分析性能的影响，探讨了水冷凝与浓硫酸吸收二者协同去溶的相关性，结果表明，OH （Q1带，带头谱线为308.520nm）的发射强度即可判别样品去溶效果。     

Sensitive Voltammetric Response of p‐Nitroaniline on Single‐Wall Carbon Nanotube‐Ionic Liquid Gel Modified Glassy Carbon Electrodes

An ionic liquid (i.e., 1‐butyl‐3‐methylimidazolium hexafluorophosphate, BMIMPF₆)‐single‐walled carbon nanotube (SWNT) gel modified glassy carbon electrode (BMIMPF₆‐SWNT/GCE) is fabricated. At it the voltammetric behavior and determination of p‐nitroaniline (PNA) is explored. PNA can exhibit a sensitive cathodic peak at ?0.70 V (vs. SCE) in pH 7.0 phosphate buffer solution on the electrode, resulting from the irreversible reduction of PNA. Under the optimized conditions, the peak current is linear to PNA concentration over the range of 1.0×10^?8–7.0×10^?6 M, and the detection limit is 8.0×10^?9 M. The electrode can be regenerated by successive potential scan in a blank solution for about 5 times and exhibits good reproducibility. Meanwhile, the feasibility to determine other nitroaromatic compounds (NACs) with the modified electrode is also tested. It is found that the NACs studied (i.e., p‐nitroaniline, p‐nitrophenol, o‐nitrophenol, m‐nitrophenol, p‐nitrobenzoic acid, and nitrobenzene) can all cause sensitive cathodic peaks under the conditions, but their peak potentials and peak currents are different to some extent. Their peak currents and concentrations show linear relationships in concentration ranges with about 3 orders of magnitude. The detection limits are 8.0×10^?9 M for p‐nitroaniline, 2.0×10^?9 M for p‐nitrophenol, 5.0×10^?9 M for o‐nitrophenol, 5.0×10^?9 M for m‐nitrophenol, 2.0×10^?8 M for p‐nitrobenzoic acid and 8.0×10^?9 M for nitrobenzene respectively. The BMIMPF₆‐SWNT/GCE is applied to the determination of NACs in lake water.     

三芳基膦配体的合成研究

从间溴苯酚出发, 利用新的合成方法经五步反应合成了一系列具有不同烷氧基的芳基膦配体. 改进后的方法可方便地通用于在苯环上具有各种不同基团基的膦配体衍生物的合成, 且有原料易得、操作简单、产率较高的优点.     

溶剂热法制备Ag/TiO2纳米材料及其光催化性能

以乙醇为溶剂, 钛酸四丁酯为前驱体, 用溶剂热法制备了Ag表面修饰的负载型纳米二氧化钛光催化剂. 利用X射线衍射(XRD)、N₂吸附-脱附(BET)、透射电子显微镜(TEM)、X射线光电子能谱(XPS)、紫外-可见(UV-Vis)光谱等技术对其进行了系统的表征, 以亚甲基蓝(MB)溶液的脱色降解为模型反应, 考察了不同Ag含量样品的光催化性能. 结果表明: 用溶剂热法制备的样品中TiO₂皆为锐钛矿相, 金属Ag颗粒沉积在TiO₂表面, 粒径为2 nm左右, 比表面积较溶胶凝胶法制备的样品大大增加, 最高可达151.44 m²·g^-1; UV-Vis光谱和光催化实验表明: Ag修饰使TiO₂对光的吸收能力大大增强, 吸收带边红移至可见光区, 亚甲基蓝在该复合材料上的光催化降解反应遵循一级反应动力学模型; 溶剂热法制备样品的光催化性能明显好于溶胶凝胶法制备的样品, 在紫外光和可见光下, Ag摩尔分数为5%的样品表现出最佳的光催化活性.     

Calix [ 4 ] arene Polyaza Derivatives： Novel Effective Neutral Receptors for Cations and α-Amino Acids

IntroductionCalixarenes are one of the most important supra-molecular building blocks, which can be modified byintroducing different functional and/or structural groupsto create a specific interaction between the host and thetarget molecules, such as meta…