Syntheses, Crystal Structures and Properties of Two Supramolecules Assembled from Weak Interactions

Two complexes, [Cu2(Htdb)4(H2O)2] (1) and [Cd(bipy)2(Hmcmbc)2] (2) (H2tdb = 2,2-thiodibenzoic acid, H2mcmbc = m-(carboxyl-methyloxy)-benzenecarboxylic acid, bipy = 4,4'-bipyridine), have been prepared, and were characterized by elemental analysis, FT-IR and single-crystal X-ray diffraction. Structures indicate that complex 1 is a single molecule, and 2 is a one-dimensional chain. Their two-and three-dimensional frameworks are constructed through hydrogen bonding, π…π or C–H…π stacking, and such other weak interactions. The cyclic voltametric behavior of complex 1 and luminescence property of complex 2 were investigated. 1 belongs to the triclinic system, space group P with a = 7.8607(6), b = 11.7619(9), c = 15.3481(12) , α = 109.3670(10), β = 92.4420(10), γ = 92.0450(10)°, V = 1335.65(18) 3, Mr = 1256.26, Dc = 1.5619(2) g/cm3, F(000) = 642, μ = 1.029 mm–1, Z = 1, the final R = 0.0289 and wR = 0.0763 for 5199 observed reflections with I > 2σ(I). Complex 2 crystallizes in triclinic, space group P with a = 9.6378(10), b = 9.7508(10), c = 19.055(2) , α = 88.7020(10), β = 80.5260(10), γ = 69.2000(10)o, V = 1649.9(3) 3, Mr = 815.07, Dc = 1.641 g/cm3, μ = 0.732 mm-1, F(000) = 828, Z = 2, the final R = 0.0511 and wR = 0.1149 for 4729 observed reflections (I > 2σ(I)).     

中药普乐安片质量标准研究

建立中药普乐安片的质量标准.采用TLC法对普乐安片中主要有效成分山奈酚-3-O-β-D-(2-O-β-D-葡萄糖基)吡喃葡萄糖苷(KMP)进行定性鉴别.采用HPLC法对普乐安片中主要有效成分山奈酚-3,4′-双-O-β-D-葡萄糖苷(KMG)和山奈酚-3-O-β-D-(2-O-β-D-葡萄糖基)吡喃葡萄糖苷进行含量测定...     

铽-环丙沙星-SDS敏化荧光猝灭法检测雷公藤红素

在pH=9.26的氨-氯化铵缓冲溶液中,铽Ⅲ与环丙沙星反应形成络合物,而后加入十二烷基硫酸钠(SDS)形成了三元体系,其最佳激发、发射波长分别为λex= 330nm、λem=545 nm.在该反应体系中加入适量雷公藤红素溶液,铽Ⅲ与环丙沙星络合物的激发、发射波长位置不变,但荧光强度有规律下降.利用这一现象,建立了测定雷...     

分子印迹整体柱在样品前处理及色谱分析中的应用

分子印迹整体柱(MIPMC)结合了分子印迹聚合物的立体选择性高和整体柱制备简单、柱压低以及传质速率快等优点,是一种极具应用潜力的样品前处理介质和色谱固定相.该文详细介绍了分子印迹整体柱的制备方法,综述了近年分子印迹整体柱在样品前处理及色谱分析中的应用进展,并对其发展趋势做了展望.     

纳米TiO_2改性蚕丝丝素蛋白膜的研究

用溶胶凝胶法制备纳米TiO2改性再生蚕丝丝素蛋白膜.该丝素膜机械强度提高,在水中溶失率下降.UV、AFM、SEM测试的结果表明,丝素中纳米TiO2粒径约为80 nm,纳米粒子在丝素膜中分布均匀;XRD、FTIR测试结果表明,纳米TiO2的加入,可使改性丝素膜的结晶结构从SilkⅠ向SilkⅡ转化,其结晶度也随之提高;TGA测试表明改性丝素膜的热转变温度比纯丝素膜有所改变.     

CH4-nFn(n=1～3)与CH3氢抽提反应微观动力学的理论研究

采用量子化学的QCISD(T)/6-311 G(d,p)//BHandHLYP/6-311G(d,p)方法研究了氟代甲烷CH4-nFn(n=1~3)与CH3自由基氢抽提反应的微观动力学性质.并利用Polyrate程序分别计算了3个反应在200~3000K范围内的速率常数.计算结果表明,R1a,R2a和R3三个反应路径的反应能量分别为-12.7,-9.5和11.8kJ/mol,相应的能垒依次为67.0,62.2和67.5kJ/mol.在437K时,kCVT/SCT分别为6.72×10-19,8.01×10-18和8.82×10-20cm3/(molecule.s).计算结果还表明,在低温段反应的量子隧道效应显著,在计算温度范围内变分效应对反应速率常数的影响可以忽略.     

自动回流萃取-MPT全谱仪测定航空润滑油中磨损金属的含量

将萃取与回流相结合, 建立了一种处理航空润滑油中磨损金属的新方法, 并用MPT全谱仪对磨损金属含量进行了同时检测. 该方法基本上实现了样品处理的全自动化,克服了常用方法的部分缺点, 对Zn, Cd, Cu, Fe和Pb的检出限(3σ)分别为0.084, 0.043, 0.022, 0.052和0.064 μg/g; 相对标准偏差均小于5%(n=5); 回收率为94.5%~107.4%. 对3个润滑油样品的检测结果令人满意.     

一种加成固化型热固性树脂PN-PAA固化过程和热稳定性研究

研究了炔丙基醚化酚醛树脂(PN)与聚芳基乙炔树脂(PAA)的反应性共混物(以下简称PN-PAA共混树脂)的相容性,并对共混树脂的固化过程和固化物的耐热性进行了表征.相态、DSC、SEM、TEM等测试结果均表明共混树脂及其固化物是完全相容的均相体系.凝胶时间、粘度、DSC等结果表明共混树脂固化工艺性优良,适合多种成型工艺(如RTM),显著改善了PAA树脂的固化工艺缺陷.DMA、TGA等分析表明共混树脂固化物具有很高的耐热性,可作为新型的防热复合材料和高温结构材料的基体.     

正交相MoO3的制备、表征及其电化学嵌锂性质

用化学沉淀-水热法在较低的温度下制备了片状正交相MoO3,由XRD、FT-IR、XPS和SEM表征了产物的相态、结构、成分和形貌。电化学测试表明,在0.1mA.cm-2的电流密度和1.2~3.5V电压范围,其初始放电容量为663mA.h.g-1,有望成为理想的锂离子插层材料。     

Synthesis and Bioactivity of Novel Fluorinated Heteroaromatic Ureas

In order to find new urea cytokinins, a series of novel fluorinated heteroaromatic ureas have been designed and synthesized. The crystal structure of 3g was further determined by single crystal X-ray diffraction to obtain the structural feature of this class of urea compounds. The preliminary bioassay showed that some title compounds have good cytokinin activity.