Stabilization of High‐Valence Ruthenium with Silicotungstate Ligands: Preparation,Structural Characterization,and Redox Studies of Ruthenium(III)‐Substituted α‐Keggin‐Type Silicotungstates with Pyridine Ligands, [SiW11O39RuIII(Py)]5−

Ruthenium(III)‐substituted α‐Keggin‐type silicotungstates with pyridine‐based ligands, [SiW₁₁O₃₉Ru^III(Py)]^5?, (Py: pyridine ( 1 ), 4‐pyridine‐carboxylic acid ( 2 ), 4,4′‐bipyridine ( 3 ), 4‐pyridine‐acetamide ( 4 ), and 4‐pyridine‐methanol ( 5 )) were prepared by reacting [SiW₁₁O₃₉Ru^III(H₂O)]^5? with the pyridine derivatives in water at 80 °C and then isolated as their hydrated cesium salts. These compounds were characterized using cyclic voltammetry (CV), UV/Vis, IR, and ¹H NMR spectroscopy, elemental analysis, titration, and X‐ray absorption near‐edge structure (XANES) analysis (Ru K‐edge and L₃‐edge). Single‐crystal X‐ray analysis of compounds 2 , 3 , and 4 revealed that Ru^III was incorporated in the α‐Keggin framework and was coordinated by pyridine derivatives through a Ru? N bond. In the solid state, compounds 2 and 3 formed a dimer through π? π interaction of the pyridine moieties, whereas they existed as monomers in solution. CV indicated that the incorporated Ru^III–Py was reversibly oxidized into the Ru^IV–Py derivative and reduced into the Ru^II–Py derivative.     

Mononuclear Water Oxidation Catalysts

Recently, several mononuclear water oxidation catalysts have been reported, a breakthrough considering the dogma that at least two metal sites were required to oxidize water efficiently. In this Review various mononuclear catalysts which have been reported in the last five years are reviewed, as well as their implementation in prototype devices that allow dioxygen formation to be coupled to dihydrogen production will be discussed.     

Simultaneous analysis of several synthetic cannabinoids,THC, CBD and CBN,in hair by ultra‐high performance liquid chromatography tandem mass spectrometry. Method validation and application to real samples

A simple procedure for the quantitative detection of JWH‐018, JWH‐073, JWH 200, JWH‐250, HU‐210, Δ⁹‐tetrahydrocannabinol (THC), cannabidiol (CBD) and cannabinol (CBN) in hair has been developed and fully validated. After digestion with NaOH and liquid–liquid extraction, the separation was performed with an ultra‐high performance liquid chromatography system coupled to a triple quadrupole mass spectrometer operating in the selected reaction monitoring mode. The absence of matrix interferents, together with excellent repeatability of both retention times and relative abundances of diagnostic transitions, allowed the correct identification of all analytes tested. The method was linear in two different intervals at low and high concentration, with correlation coefficient values between 0.9933 and 0.9991. Quantitation limits ranged from 0.07 pg/mg for JWH‐200 up to 18 pg/mg for CBD The present method for the determination of several cannabinoids in hair proved to be simple, fast, specific and sensitive. The method was successfully applied to the analysis of 179 real samples collected from proven consumers of Cannabis, among which 14 were found positive to at least one synthetic cannabinoid. Copyright © 2012 John Wiley & Sons, Ltd.     

二氧化钛含量对铈稳定立方氧化锆陶瓷的性能影响

本文用无压烧结法成功制备了高硬度的立方氧化锆陶瓷,研究了氧化锆陶瓷的物相,Vickers硬度,显微结构,相对密度等性能,主要分析了TiO2添加量对Zr0.8Ce0.2O2陶瓷硬度和相对密度的影响。结果表明:烧结助剂TiO2可以有效抑制陶瓷晶粒异常生长,加快气孔排除,促进氧化锆陶瓷烧结致密化,提高陶瓷硬度。最高维氏硬度为20.2 GPa,最高相对密度达到了99.8%。     

用于测量亚硝酸的长光程吸收光谱仪的研制

This article has been retracted at the request of the authors.     

糖苷配合物与DNA作用机理的电化学研究进展

本文综述了糖苷配合物的合成、表征、生物功能及糖化学研究现状，并对糖苷功能配合物与DNA的作用机理及生物功能的电分析化学研究进行了探讨。着重讨论了应用电分析化学、谱学方法、单晶X-射线衍射分析来研究糖苷功能配合物。引用文献39篇。     

煤显微组分分子结构模型的量子化学研究

采用分子力学和半经验量子化学方法，研究了神木煤显微组分的分子结构模型，比较了镜质组和惰质组分子模型的能量构成、不同类型键的键长和键裂解能。研究结果表明，扭转能和范德华能是分子中的主要作用力，取代基对体系能量有明显影响，烷基取代基使体系能量增加，而苯基取代基使体系能量降低；脂肪C—C键长比芳香C—C键长长，说明脂肪C—C在受热过程中比芳香C—C更容易断裂分解。对各键裂解能的计算结果表明，Car—Cal键的裂解能高于Cal—Cal，Car—O醚键的裂解能高于Cal—O醚键。而惰质组结构模型中除C—O醚键外，各键的裂解能均高于镜质组，说明惰质组结构模型比镜质组有较高的热稳定性。     

反相高效液相色谱法测定肾复康胶囊中的野黄芩苷和芦丁

建立了肾复康胶囊中野黄芩苷和芦丁的反相高效液相色谱测定方法。以甲醇-水为提取溶剂,采用超声提取法对样品进行前处理。以0.02 mol/L磷酸二氢钾缓冲溶液(含1.0％（体积分数）冰醋酸)-甲醇（体积比为63∶37）为流动相,于330 nm波长下检测,肾复康提取液中野黄芩苷和芦丁可达基线分离,分析时间在20 min内。野黄芩苷和芦丁在10 ~300 mg/L内,其峰面积与浓度之间线性关系良好,目标物的加标回收率大于98％。该方法适用于肾复康胶囊及相关药材中野黄芩苷和芦丁黄酮类化合物的测定和质量控制。     

曲线拟合定量法在高效液相色谱手性分离中的应用

 首次将曲线拟合定量法用于解决高效液相色谱手性分离中重叠峰的定量问题。通过比较百树菊酯 8个立体异构体的实验谱图和拟合谱图 ,证明曲线拟合定量法与传统的中切法相比 ,可获得更令人满意的结果。     

固相萃取-高效液相色谱-质谱联机在线分析水中痕量除草剂

建立了饮用水中痕量除草剂的SPE－LC－MS联机测试方法,该方法仅用45min就可完成水样中7种除草剂（阿特法津,西草净,西码净,杀草净,敌稗,乙草胺,甲磺隆）的分析,检测限低于欧共体所要求的饮用水标准（单种农药浓度小于0．1ug/L）。比起液液萃取,离线SPE等其他前处理方法,在线SPE的结果的重现性和精密度方面大大优于前者,环境水样分析时间大大减少（所需时间为液液萃取的、1／60,离线SPE的1／20）,而且更安全性和可靠。我们已在华北某地的地表水和地下水中检测出阿特拉津（1．9ug/L)和乙草胺（1．64ug/L）。