双核锌配位化合物[Zn(C15H8O7S)(DMSO)]2•H2O的合成和晶体结构及光致发光性能研究

以白杨素为先导化合物, 对其进行磺化, 磺化衍生物与锌络合, 在含水10%的二甲基亚砜(DMSO)溶液中重结晶, 得双核锌配位化合物[Zn(C₁₅H₈O₇S)(DMSO)]₂•H₂O. 采用IR, ¹H NMR, DSC-TGA, 元素分析和X射线单晶衍射法对标题化合物进行了表征和晶体结构测定. 标题化合物属正交晶系, 空间群Pbcn, Zn(II)的配位数为5, 配位原子均为氧原子, 每个五配位的锌都具有四方锥型的配位构型, 被2个配体5-羟基氧负离子-7-羟基黄酮-6-磺酸根的5-羟基氧负离子桥联, 形成了一个中心Zn₂O₂的菱形平面. 水溶性白杨素黄酮配体与Zn(II)通过氢键、π-π堆积和配位作用自组装形成了一个三维结构的超分子化合物. 差示扫描量热分析(DSC-TGA)结果表明,标题化合物配体骨架分解温度为518.26 ℃. 同时, 标题化合物固体具有较强的光致发光现象, 在λ_ex＝423 nm条件下可发出λ_em＝488 nm的黄色荧光, 并对其发光机制进行了探讨.     

使用滴液式气体发生器制备乙炔

采用恒压分液漏斗和蒸馏烧瓶组成的装置,饱和食盐水与电石反应是实验室制备乙炔的常用方法。该实验产生糊状Ca(OH)₂沉淀,存在反应速率过快、无法控制反应进程、产生气流不平稳、泡沫随气体冲出堵塞导管等问题。利用滴液式气体发生器,在反应容器中加入7 mm玻璃珠与电石混合,以10%氯化铵溶液为反应液,解决了实验室制备乙炔存在的问题,同时也提高了制备乙炔的产率。     

Synthesis,Crystal Structure and Antitumor Activity of Tectochrysin-6-sulfonate

In order to enhance water-solubility and biological utilization rate of tectochrysin,sodium 5-hydroxyl-7-methoxyflavone-6-sulfonate(1) was synthesized and its structure was identified on the basis of 1 H NMR,FT-IR and elemental analysis.5-Hydroxyl-7-methoxyflavone-6-sulfonate was assembled with Ni(II) or Mn(II),hexaquanickel(II) bis(5-hydroxyl-7-methoxyflavone-6-sulfonate) tetrahydrate(2) and hexaquamanganese(II) bis(5-hydroxyl-7-methoxyflavone-6-sulfonate) tetrahydrate(3) were obtained and characterized by IR spectroscopy.The crystal structures of 2 and 3 were determined by X-ray single-crystal diffraction analysis.The results showed that 2 and 3 are isomorphous crystals and crystallize in monoclinic crystal system,space group C2/c.In 2 and 3,the supramolecular structures are organized into hydrophilic and hydrophobic regions.Hydrophilic regions are generated by O–H???O hydrogen bonds among sulfonate groups,latticed water molecules and coordinated water molecules.The π-π stacking interactions assemble the flavone skeletons into columns and these columns form hydrophobic regions.The sulfonate groups play an important role as a bridge of the hydrophilic and hydrophobic regions as well as the inorganic and organic components.Three-dimensional networks of 2 and 3 are furnished by extensive array of hydrogen bonds,π-π stacking interactions and electrostatic interactions.The anti-proliferative activities of 1~3 in vitro against human leukemia cells K562 and human lung cancer cells A549 were evaluated by the standard MTT assay.The pharmacological activity results showed that the introduction of sulfonic acid groups enhanced the antitumor activity of tectochrysin.     

Syntheses and Crystal Structures of [Na(H_2O)](C_(17)H_(13)O_6SO_3)·2H_2O and [Ni(H_2O)_6](C_(17)H_(13)O_6SO_3)_2·4H_2O

Introduction Flavonoids exist widely in edible plants, and have pharmacological activity. They played a major role in the successful medical treatments at ancient times, and their uses have been persevered up to now.1-3 Flavonoid sulfates were found in a large number of plant species. They occupy an important position in the field of natu-ral products chemistry since they provide structures consisted of organic and inorganic components. The pharmacological assay revealed that flavonoid sulfat…     

某型陀螺仪自然贮存寿命评估与加速寿命试验时间预估

某型陀螺仪是影响武器控制舱贮存寿命的薄弱环节,针对历年统计的陀螺仪的成败型、不完全故障数据,将"保序回归"和"变样本Pearson?2拟合优度检验与极小卡方估计"相结合,得到了其寿命分布函数。结果显示,I型极大值和威布尔分布适用于陀螺仪的寿命分布,但I型极大值不具有可加速性,因而选择威布尔分布作为寿命分布。根据统计数据计算,得到了置信度0.90和可靠度0.95时陀螺仪自然贮存寿命为22.30年,得到了陀螺仪在90℃下的加速系数K=7.2695,预估了2009年和2011年生产的陀螺仪加速寿命试验时间分别为8.25月和11.56月,对加速寿命试验时间规划、经费预算具有工程实际意义。     

等厚干涉法测量盐度

根据等厚干涉的原理,本文提出了一种通过测量水质的折射率来测定盐度的光学方法。测量误差低于3％。     

圆管内大液气比下液雾在高温气流中蒸发特性的研究

本文获得了液雾在过热蒸发状态下的液气两相能量方程,给合运动学方程、粒径分布及轨道模型,组成了描述液雾的完整数学方程组。提出将时间变量隐含在空间变量中来克服由于大液气比引起的“物性漂移”,考虑了壁面捕获。计算结果表明:大滴径粒子与小滴径粒子,参数变化具有不同的特征,并对气相温度场的模型计算值与实验值进行了比较.     

应用耗散结构理论研究两相流动不稳定性的探讨

本文论证指出:两相流动动力学不稳定性是一种耗散结构。这一结论将非线性非平衡态热力学引入了两相流动不稳定性研究之中,从而阐明了不稳定性发生的原因和机理,并且找到了两相流动不稳定性的直接判据——超熵(1/2δ~2s)(它是非线性非平衡系统的Lyapounov函数)。本文得出了线性非平衡区的判别式和非线性区的一些初步结果,并阐述了在实际应用中对两相流动不稳定性进行判别的具体步骤及本文方法的优越性。     

电喷雾质谱法研究细胞色素Tb5及其F35Y突变体蛋白 肽链和辅基的相互作用

本文通过牛肝线粒体细胞色素Tb5和它的F35Y突变体蛋白相对分子质量的外标法测定,得到细胞色素Tb5全蛋白的相对分子质量为10077.5脱辅基蛋白的相对分子质量为9461.4F35Y突变体蛋白的相对分子质量为10093.6,它的脱辅基蛋白的相对分子质量为9477.5,不同nozzle电压下的电喷雾质谱结果表明,该电压的大小明显影响蛋白肽链与血红素辅基之间的非共价结合,随着电压的降低,全蛋白谱峰的强度逐渐增大,然而,过低的电压导致了Na^+,K^+离子加合峰相对强度的增加,而不利于谱图分析。同时,考察到细胞色素Tb5在甲醇溶液和酸性溶液中的变性行为,因此选择nozzle电压70V,10%的甲醇水溶液和pH=7为得到全蛋白质谱峰的最佳条件。相同实验条件下得到的野生型CytTb5和F35Y突变体全蛋白的质谱峰相比较,其相对丰度有悬殊的差异,表明F35Y突变体蛋白的血红素结合能力明显低于野生型蛋白。通过解离出的Hemeb的分子离子峰进行解析,证明铁仍以三价离子存在于血红素辅基中。