β-环糊精交联聚合物树脂相分光光度法测定水中痕量汞

以β-环糊精和环氧氯丙烷为原料合成了环糊精聚合树脂,将其作为显色剂2-[5-溴-(2-吡啶偶氮)]-5-二乙氨基苯酚的载体,采用β-环糊精-2-[5-溴-(2-吡啶偶氮)]-5-二乙氨基苯酚树脂相分光光度法测定微量汞.配合物的最大吸收波长为585nm,表观摩尔吸光系数为8.17×105L/mol·cm,汞含量在0～10μg/25mL范围内服从比尔定律,线性回归方程:y=0.0013 0.0163x,相关系数r=0.9994,加标回收率为98.5%～101.0%,与双硫腙法相比无显著性差异.该方法已用于工业废水中痕量汞的测定,结果令人满意.     

新型杀菌剂氟吗啉在黄瓜植株体内的吸收传导行为

利用生物测定技术和高效液相色谱法研究了氟吗啉在黄瓜植株体内的吸收、传导和分布行为及其机制. 结果表明, 氟吗啉能被黄瓜植株被动吸收, 并通过木质部在体内传导和分布.     

超分子钴(Ⅱ)配合物[CoL(H2O)2]n的合成与结构表征

A mononuclear Cobalt(Ⅱ) complex [CoL(H₂O)₂]_n (H₂L: 4,4′,6,6′-Tetrabromo-2,2′-[ethylenedioxybis(nitrilomethylidyne)]diphenol), has been synthesized and structurally characterized by elemental analysis, IR and X-ray diffraction single crystal structure analysis. The crystal of the complex belongs to monoclinic space group P2₁/c with a=2.516 8(3) nm, b=1.023 43(18) nm, c=0.789 17(14) nm, β=91.375(2)°, V=2.032 1(5) nm³, Z=4, D_c=2.317 Mg·m^-3, μ(Mo Kα)=8.747 mm^-1, F(000)=1 356, R₁=0.049 7, wR₂=0.110 4. The crystal structure of [CoL(H₂O)₂]_n indicates that the complex consists of one cobalt(Ⅱ) atom, one L^2- unit and two coordinated water molecules, and the coordination number of the cobalt(Ⅱ) atom is six. One-dimensional chain supramolecular structure is formed by intermolecular hydrogen bonds and π-π stacking of neighboring benzene rings. CCDC: 652649.     

3,5—二溴水杨醛—4—BSDP—CTMAB荧光光度法测定痕量铝

基于Al~(3+)与3,5-二溴水杨醛-4-氨基安替比林(BSDP)-溴化十六烷基三甲铵(CTMAB)形成络合物导致体系荧光增敏的特性,提出了一种测定痕量铝的新荧光方法。在pH 4.5～5.5的乙酸铵缓冲溶液及CTMAB存在下,铝与BSDP形成1:1的络合物。在λ_(ex)=375nm、λ_(em)=510nm条件下,体系产生的荧光增敏程度最大,铝量的线性范围为0.06～0.60μg/25ml,检出限为0.20ng·ml~(-1)。方法用于废水和合金钢中的痕量铝测定,结果满意。     

Synthesis of Pharmaceutical Intermediates by Toluene Benzylation over Heteropoly Acids on Different Support

Selective formation of pharmaceutical intermediates like diphenylmethane, dimethyl- diphenylmethane, benzyl toluene and benzoic acid by liquid phase, toluene benzylation with benzyl chloride as a benzylating agent, was systematically studied over plane clay (K-10, montmorillonite), plane H-Beta, plane MFI structured titanosilicate (TS-1) and heteropoly acids [HPA, namely dodeca-tungstophosphoric acid [H3PO4.12WO3.xH2O] (TPA), dodeca-molybdo phosphoric acid ammonium salt hydrate [H12Mo12N3O40P aq] (DMAA), sodium tungstate hydrated purified [Na12WO4.2H2O] (STH)] supported on clay, H-beta and TS-1. The 20%TPA/Clay, 30%TPA/H-Beta and 30%TPA/TS-l, were observed to be the best catalyst samples over plane clay, plane H-Beta and plane TS-1. The catalyst samples are compared with respect to benzyl chloride conversion and selectivities for diphenylmethane, dimethyl-diphenylmethane, benzyl toluene and benzoic acid. The reaction follows the pseudo-first order rate power law model. The apparent rate constants are calculated and compared with the reported ones.     

交流示波极谱滴定法：溴量法在药物分析上的应用

磺胺类是消炎药,对氨基水杨酸是抗结核药,对这两类药物的含量测定,文献报道多为亚硝酸钠法,银量法等。亚硝酸钠法:指示终点的方法还不够理想,应用永停法,电极易于钝化,应用外指示剂法,由于多次外试而增加误差;银量法则终点不易观察。     

CH2F2…H2O中强π型二级氢键

通过从头计算,用较大基组６－３１１＋Ｇ(２ｄ,２ｐ),在ＭＰ２水平上计算得到ＣＨ２Ｆ２…Ｈ２Ｏ体系的优化几何构型,与实验结构一致．其中∠Ｆ…Ｈ－Ｏ＝１１６．５°,偏离普通氢键之键角达到６３．５°．为探讨产生氢键巨大弯曲的原因,采用点电荷扫描的办法,探测ＣＨ２Ｆ２…Ｈ２Ｏ体系中Ｈ２Ｏ的Ｏ原子上的两对孤电子对的方向,发现了一个强的π型二级氢键相互作用．使用这种新的相互作用方式说明了产生这一巨大氢键弯曲的原因,并且在ＭＰ４水平上使用Ｃｏｕｎｔｅｒｐｏｉｓｅ技术计算了π型二级氢键的稳定化能．     

Synthesis of a Novel Core-shell Type Acrylic-polyurethane Hybrid Emulsion Containing Siloxane and Fluorine as well as Water and the Oil Resistances of Cured Film

Aqueous acrylic-polyurethane dispersions have become one of the major types of materials used in coating, paint and adhesive industries, because of excellent properties and environmental advantages1-5. However, some properties for cured film such as water…     

The Chemistry of Tetrafluoroallene： One－pot Synthesis of Trifluoromethylindolizines from 1,3－Diiodo－1,1,3,3－tetrafluoropropane by 1,3－Dipolar Cycloaddition

Heating a mixture of 1, 3-diiodo-1, 1, 3, 3-tetrafluoropropane (2), K2CO3, pyridinium bromides (3) in CH3CN at 65℃ for 10 h gives the corresponding trifluoromethylindolizines.     

盐酸环丙沙星的合成

以３－氯－４－氟苯胺为起始原料，经六步反应合成盐酸环丙沙星，总收率达４２．３％，高于现有文献报道值。经元素分析，红外光谱和核磁共振谱确认了产物的结构。