一种锌配合物用于炭疽生物标志物的检测

采用溶剂热合成方法,合成了一种新型金属配位聚合物{[Zn₂(L)(H₂O)(DMA)]·DMA·2.3H₂O}_n (1),其中L^4-为完全脱去质子的N,N''-二(4-羧基苄基)-5-氨基间苯二甲酸,DMA为N,N-二甲基乙酰胺。单晶X射线衍射结果显示,该配合物属于三斜晶系,空间群为P$overline{1}$,a=0.989 6(5) nm,b=1.370 5(5) nm,c=1.382 1(5) nm,α=80.067(5)°,β=76.729(5)°,γ=76.611(5)°,结构是由二维金属有机层通过π…π相互作用而扩展成的三维超分子骨架。红外光谱验证了锌离子与L^4-配体成功配位。粉末X射线衍射(PXRD)实验证实了配合物1具有较高的纯度。热重分析结果显示配合物1在室温至416.9 ℃区间内具有较好的热稳定性。在273 nm的激发光下,配合物1在437 nm处有较强的荧光发射,可以在30 s内快速检测乙醇溶液中的炭疽生物标志物——吡啶-2,6-二甲酸,具有选择性高、抗干扰能力强、检测限低(约为15 μmol·L^-1)等特点。结合PXRD图和紫外可见吸收光谱揭示了其检测机理为晶体骨架坍塌而诱导的荧光猝灭。     

三光气与酚制备三氯甲氧基甲酸芳酯研究

研究了不同取代酚与三光气的反应,得到七种未见报道的新化合物,以IR、MS、1H NMR、13C NMR对产物进行了表征,并探索得到合适的反应催化剂、反应物浓度配比、反应时间,讨论了酚上不同取代基对反应的影响,收率在78.5～90.5%之间。     

Effects of the laser surface treatment on the mechanical properties of CuZr-based bulk metallic glasses

Surfaces of three types of CuZr-based bulk metallic glasses (BMGs) were modified by laser surface treatment (LST), and the influence of the treatment on structure and mechanical properties of these alloys was investigated. The phase structure of as-cast and laser-treated samples was characterized by XRD and the morphology of the alloys after fracture was examined by SEM. The compressive plasticity of treated Cu47.5Zr47.5Al5 and Cu46.5Zr47.5Al5Co1 BMGs can be improved from 0.5% to 2.0% and from 1.2% to 5.7% respectively compared with the as-cast ones, while (Cu0.55Zr0.40Al0.05)99Er1 BMG shows insignificant change of plasticity. The improvement in plasticity is attributed to induced crystallization of B2 CuZr phase in the treated surface zone of selected metallic glasses.     

Optical bistability based on surface plasmon coupled between two noble metal films involving Kerr materials

We successfully investigate an optical bistability phenomenon in a layered structure consisting of Kretschmann configuration involving the Kerr-type nonlinear and the silver film. Pure theoretical approaches are employed to investigate that the surface plasmon could easily be coupled and both the reflection and transmission curves versus the incident intensity forms optical bistability. The transmission curves are greatly influenced by the thickness of the second silver film. These results may be useful for designing novel surface plasmon-based optical devices and will be essential for future classical and quantum information processes.     

中德化学启蒙教材有机内容比较

就化学启蒙教育阶段有机化学教学内容,将德国的《今日化学SⅠ》、国内的沪教版、人教版、鲁教版4套教材,从知识内容的选取、组织呈现等角度进行了比较,并在实验设计、作业设计、拓展学习3方面向教材编写和教学实践提出了建议。     

Legendre函数加权的声纳宽频带恒定束宽波束特性分析*

为了处理水声信号,声纳阵列通常需要形成宽频带恒定束宽的波束。采用两种阵元加权方法分析二维圆弧形恒定束宽换能器声纳阵列:球面Legendre函数加权方法和柱面Legendre函数加权方法。分别对球面阵、柱面阵和平面阵这三种几何结构的声纳阵列进行分析,并且计算波束宽度和波束方向。结果表明,在宽频带范围内,除了柱面Legendre函数加权的球面阵之外,其余Legendre函数加权的声纳阵列均能利用简单的、不随频率变化的阵元权重和阵元延时,形成恒定束宽的波束,并且具有较小的旁瓣,此外波束方向与预设方向也较为一致。相对于其他恒定束宽波束形成方法,Legendre函数加权方法能利用较低的计算复杂度来实现良好的宽频带恒定束宽的波束特性。     

黄芩中黄芩苷的亚临界水提取及高效液相色谱分析

建立了黄芩药材中黄芩苷的亚临界水提取 高效液相色谱测定方法。分别考察了温度、压力、提取时间、提取物颗粒度、溶剂比等因素对提取量的影响,并与有机溶剂提取法比较。结果表明,当两者具有相同的提取效果时,亚临界水提取法的提取时间及提取溶剂的消耗量大大减少,避免了使用有机溶剂造成的污染。黄芩苷提取最佳条件为:样品颗粒度80～100目,溶剂比0.2 mL/mg ,5 MPa,130 ℃保持10 min。并通过提取 高效液相色谱联机分析实现了对提取物的实时监测。该技术有望成为从中药材中提取脂溶性成分的有效方法。     

Rejoinder for Gaining effciency via weighted estimators for multivariate failure time data

We thank all the discussants for their interesting and stimulating contributions. They have touched various aspects that have not been considered by the original articles.     

金属-半导体异质结构纳米晶的可控制备和光谱调控

本文简要综述了金属-半导体异质结构纳米晶的设计、可控制备和物性研究的相关工作.设计了异相成核与生长、选择硫化和种子介导液相外延生长3种不同的方法并以此制备了多种金属-半导体异质结构纳米晶,对其中所涉及的反应机制进行了论述,并简要探讨了金属-半导体异质结构纳米晶的热稳定性、表面等离子共振活性、荧光特性以及异质界面的电荷转移和保持能力.     

Highly Selective Synthesis of Methyl 1-Phenyl-1-(9-hydro-)fullerenylacetate

Isomerically pure methyl 1-phenyl-1-(9-hydro-)fullerenylacetat is synthesized in 75% yield by the reaction of C₆₀ with the carbanions of methyl phenylacetate in C₆H₆/THF mixed solvent under a purified N₂ atmosphere at 20°C.