螯合型二甘醇钛酸酯的合成及其催化性能研究

报导了两种新的螯合型二甘醇钛酸酯的合成方法，进行了ＩＲ和ＵＶ鉴定，并作为酯化反应催化剂催化合成了邻苯二甲酸二辛酯。研究了酯化反应转化率与反应时间、反应温度及催化剂用量的关系，探讨了催化剂结构与催化性能的关系。     

An azo dye for photodynamic therapy that is activated selectively by two-photon excitation

Two-photon photodynamic therapy (TP-PDT) is a promising approach for the treatment of cancer because of its better penetration depth and superior spatial selectivity. Here, we describe an azo group containing cyclized-cyanine derivatives (ACC1 and ACC2) as a two-photon activated, type I based photosensitizer (PS). These small-molecule and heavy atom-free organic dyes showed marked reactive oxygen species (ROS)-generating ability under physiological conditions, as well as fast loading ability into the cells and negligible dark toxicity. Live cell analyses with one- and two-photon microscopy revealed that these dyes showed higher ROS generation ability upon two-photon excitation than upon one-photon excitation via the type I process. The PSs have superior PDT properties compared to conventional Visudyne and 5-ALA under mild conditions. These characteristics allowed for precise PDT at the target region in mimic tumor spheroids, demonstrating that the developed TP PS could be useful in efficient PDT applications and in designing various PSs.

Azo containing dyes as a two-photon selective and type I based photosensitizers (PSs) were developed that exhibit excellent photodynamic therapy properties under mild condition.     

Locally enhanced relative humidity for scanning probe nanolithography

The formation of a water meniscus between a sharp tip and a solid surface is one of the prevailing requirements for scanning probe microscope (SPM)-based lithographies, such as dip-pen nanolithography (DPN) and conductive tip induced oxidation. The water meniscus functions as a medium for the oxidation of or mass transfer to the solid surface. Here we report a simple, efficient, and effective approach to enhance the local relative humidity and thus increase the size of the water meniscus by bringing a water-containing capillary tube to the proximity of the tip-surface contact area. The enhancement in local relative humidity is confirmed via an increase in the measured tip-surface adhesion forces and the widths of DPN generated parallel lines. Compared to the global control of relative humidity for the whole lithography system, the short distance between the "water reservoir" and the tip-surface contact area enables rapid increase in the local vapor pressure of water, less perturbation, and minimal erosion to the state-of-the-art electronics. As a result, most scanning probe lithography experiments at high relative humidity can now be performed in a reasonable time frame.     

Photocatalytic degradation of methylene blue on Fe3+-doped TiO2 nanoparticles under visible light irradiation

Fe³⁺-doped TiO₂ composite nanoparticles with different doping amounts were successfully synthesized using sol-gel method and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and ultravioletvisible spectroscopy (UV-Vis) diffuse reflectance spectra (DRS). The photocatalytic degradation of methylene blue was used as a model reaction to evaluate the photocatalytic activity of Fe³⁺/TiO₂ nanoparticles under visible light irradiation. The influence of doping amount of Fe³⁺ (ω: 0.00%–3.00%) on photocatalytic activities of TiO₂ was investigated. Results show that the size of Fe³⁺/TiO₂ particles decreases with the increase of the amount of Fe³⁺ and their absorption spectra are broaden and absorption intensities are also increased. Doping Fe³⁺ can control the conversion of TiO₂ from anatase to rutile. The doping amount of Fe³⁺ remarkably affects the activity of the catalyst, and the optimum efficiency occurs at about the doping amount of 0.3%. The appropriate doping of Fe³⁺ can markedly increase the catalytic activity of TiO₂ under visible light irradiation. __________ Translated from Journal of Northwest Normal University (Natural Science), 2006, 42(6): 55–56 [译自: 西北师范大学学报(自然科学版)]     

流动注射在线阴离子树脂预富集火焰原子吸收测定痕量铜

研究了以阴离子交换树脂作吸附剂的流动注射在线微柱预富集火焰原子吸收测定铜的新方法。在最佳条件下富集１５０ｓ，富集２３倍，检出限０．２μｇ／Ｌ，ＲＳＤ为１．６％，分析速度２０次／ｈ。天然水样中可能存在的离子不干扰铜的测定。所建立的方法已用于水样中痕量铜的测定。     

真珠钙驱铅实验研究

研究了真珠钙驱铅效果，给亚急性中毒的大鼠服用后，可增加铅从尿中排量，降低骨中蓄积量，对防治铅中毒有一定作用。     

Synthesis and structure of Ca(18)Li(5)In(25.07): a novel intergrowth of Li-centered in(12) icosahedral clusters and electron-precise Zintl layers

A new ternary polar intermetallic, Ca(18)Li(5)In(25.07), was obtained from high-temperature reactions of the elements in welded Nb tubes. Its crystal structure, established by single-crystal X-ray diffraction, was found to crystallize in the orthorhombic space group Cmmm (No. 65). Unit cell parameters are a = 9.9151(6) A, b = 26.432(2) A, and c = 10.2116(6) A; Z = 2. The structure of Ca(18)Li(5)In(25.07) features two distinct types of indium anionic layers. An "electron-deficient" layer is made up of Li-centered In(12) icosahedra that are interconnected by bridging planar In(4) units and In atoms. A second In(3)(5-) layer is an electron-precise Zintl layer formed by fused four-, five-, and six-membered rings of three- and four-bonded indium atoms. The two distinct layers are alternately stacked and linked into a complex three-dimensional network. Vacancies are observed to occur only at the In(12) icosahedral and the bridging indium units within the "electron-deficient" layers. Magnetic property measurements indicate that Ca(18)Li(5)In(25.07) exhibits temperature-independent paramagnetism consistent with metallic behavior. Band structure calculations were performed to elucidate the role of defects and vacancies in the electronic structure of the electron-deficient "metallic" Zintl phase.     

芥子气模拟剂2-氯乙基乙基硫醚的光催化降解

利用连续流动微反、原位红外和GC/MS等手段考察了芥子气模拟剂2-氯乙基乙基硫醚（2-CEES）在P25 TiO2上的光催化降解反应,证实CO2和H2O是这个反应的最终产物.详细的跟踪分析表明,除了CO2和H2O外,在反应的气相混合物中可检测到C2H4、CH3CHO、CH4、CO、HCl和H2S；少量小分子的羧酸、醚和砜；微量C2H5SC2H5、C2H5S2C2H5、C2H5SC2H4Cl和CH2ClCH2Cl等中间产物;在反应后的催化剂表面可检测到C2H5S2C2H5、C2H5SC2H4OH、C4H9S2C2H5和C2H5S2C2H4OH、等物.根据这些结果提出了2-CEES光催化降解的反应机理,推断2-CEES的光催化降解涉及脱氯、C－S键断裂、有机硫化物光聚合和裂解等复杂过程最终转化为CO2和H2O.认为各种硫物种在表面的积聚引起了催化剂的缓慢失活.     

铜在HOPG上电沉积过程的现场ECSTM研究

用自制的电化学扫描隧道显微镜（ＥＣＳＴＭ）现场研究Ｃｕ在ＨＯＰＧ上的电沉积过程．结果表明Ｃｕ在ＨＯＰＧ上的电沉积为三维成核的过程．当电位较低或Ｃｕ２＋离子浓度较低时，铜在本体金属生长主要沿着台阶方向．过电位较高时，铜的成核数目增加，沉积层的晶粒有所细化．同时，非现场ＥＣＳＴＭ比较研究表明，ＳＴＭ针尖对针尖局部区域的电沉积起屏蔽作用，针尖所在区域Ｃｕ的沉积速度比其它区域明显减小     

Liquid chromatography/electrospray tandem mass spectrometry method for the quantitation of fosinoprilat in human serum using automated 96-well solid-phase extraction for sample preparation

A sensitive, specific, accurate and reproducible liquid chromatography/electrospray tandem mass spectrometry method was developed and validated for the quantitation of fosinoprilat in 0.2 mL of human serum. The method employed acidification (with pH 4.0 sodium acetate buffer) of the serum samples to minimize the hydrolysis of the prodrug fosinopril to fosinoprilat prior to purification by automated 96-well solid-phase extraction. The required chromatographic separation of fosinoprilat and fosinopril was achieved isocratically on a Luna C8 analytical column (2 x 50 mm, 3 microm). The total run time was 2 min. The mobile phase contained methanol and water with 10 mM ammonium acetate. Detection was by positive ion electrospray tandem mass spectrometry. The standard curve, which ranged from 2.00 to 500 ng/mL, was fitted to a 1/x(2) weighted linear regression model. Fosinoprilat quality control (QC) samples used to determine the accuracy and precision of the method were prepared in human serum at concentrations of 5.00, 200, 400 and 1000 ng/mL. The assay accuracy was within 8% (dev). The intra- and inter-assay precisions were within 6 and 3% (RSD), respectively. Fosinopril QC samples used to gauge the rate of hydrolysis of fosinopril to fosinoprilat during the assay procedure were prepared in human serum at 500 ng/mL. The hydrolysis of fosinopril to fosinoprilat was 相似文献