核磁共振法测定高聚物的结构—核磁共振二维谱

介绍了核磁共振(NMR)波谱,尤其是核磁共振二维谱(2D NMR)在最近几年内的进展。内容包括怎样用NMR测定高聚物的序列分布、共聚物结构、聚合物的混溶性、聚合物液晶的取向度、分子量、短链度和长链支化度、凝聚态高聚物的多相结构等。     

自制苯乙烯-丙烯酸乙酯共聚物与PEG20M复合萃取涂层用于洗涤制品中1,4-氧杂环己烷的测定

采用顶空固相微萃取-毛细管气相色谱联用技术测定了洗涤制品中的1,4-二氧杂环己烷.使用自制的萃取头(苯乙烯-丙烯酸乙酯共聚物与PEG20M复合)于顶空平衡温度80℃下萃取样品40 min.萃取物用内壁涂有SE-30固定液的石英毛细管柱分离,外标法定量.1,4-二氧杂环己烷含量为0.35～120 μg/g时,其峰面积与含量呈良好的线性关系(r=0.999 8);回收率为98.7%～102%;相对标准偏差(n=5)为9.33%.     

水杨酸与烟草铜锌超氧化物歧化酶的相互作用

利用邻苯三酚自氧化法监测了磷酸盐缓冲体系中水杨酸（SA）对超氧化物歧化酶（SOD）活力的影响。通过荧光光谱法研究了水杨酸与超氧化物歧化酶的相互作用机制，求得两者结合的形成常数和配位数，使用Forster非辐射能量转移技术求出了两者的结合位置距色氨酸残基间的距离为2.60nm。     

尖吻蝮蛇毒抗凝血因子(ACF)含量和钙离子含量的定量测定及钙离子结合位点的初步研究

由紫外光谱法测定蛋白质浓度,用ICP测定Ca含量,从而确定一个ACF分子中含一个钙离子.ACF中分子中除一个高亲和性钙结合位点外,至少还有一个低亲和性钙结合位点,只有当过量钙离子存在时,才可能在低亲和性钙结合位点上进一步结合钙离子.Tb~(3+)具有比Ca~(2+)离子更强的键合ACF能力,能定量结合在ACF中的两个位点上,且能全部取代ACF中Ca~(2+).文中提及的金属离子对ACF的抗凝血活性没有显著的影响.     

Synthesis,crystal structure and spectroscopic characterization of a hydrogen-bonded 1D copper(II) complex

Novel 1:2 and 1:1 (M:L) copper(II) complexes have been prepared from the tridentate ligand 2-(1-methyl-2-aza-5-oxapentyl)phenol (H₂L¹). The crystal structure of [Cu(HL¹)₂] (1) exhibits a noncentrosymmetric square-planar geometry with a slightly tetrahedral distortion. The Cu^II atom is coordinated by two amino N and two phenoxo O atoms of two (HL¹)^– ligands. The phenoxo and the alkoxy groups are involved in two strong intramolecular hydrogen bonds. The coordination moieties are further connected to a 1D linear structure by the action of intermolecular hydrogen bonds between the alkoxyl and the amino groups. The importance of steric hindrance introduced by the methyl group in the molecular structure and the packing of the complex molecules has been demonstrated. The e.p.r. parameters of (1) have been obtained: g = 2.231, g = 2.005, g _iso = 2.080, A = 185.0 G, A _iso = 86.5 G, A = (3A _iso – A )/2 = 37.3 G. These results confirm a distorted square planar stereochemistry with a ( )¹ ground state.     

Notable shift of ultraviolet intensity on Sn-doped ZnO nanostructure fabricated by sol–gel method

Sn-doped ZnO (SZO) thin films are deposited by sol–gel dip-coating method with Sn content at 0 at.% and 1–15 at.% with an increment of 2 at.%. The structure and luminescence of the films are investigated. X-ray diffraction results indicate that all the SZO samples show preferential orientation along the (002) direction, and the scanning electron microscope exhibits that the surface morphology of the films change from nanoparticles to nanorods with increasing Sn concentration. X-ray photoelectron spectroscopy reveals that Sn exists as valence of +4 in the matrix. The photoluminescence peaks at 381 and 398 nm are observed in all the samples. The ratio of intensity of peak at 381 nm to that of peak at 398 nm differed markedly. The intensity of peak at 398 nm might be due to the response for the Sn atoms, while the intensity of peak at 381 nm is probably related to the quantum size effect.     

Design of a small-sized expanded coaxial line antenna at L-band

为了减小常规L波段高功率微波测量接收天线的结构尺寸及增益,设计了一种基于轴向缝隙馈电的小型化同轴扩张型天线.通过理论分析和数值模拟,选择了较优的结构尺寸,得到天线的增益及方向图特性:在1.3～1.6 GHz范围内,增益从-2.0 dBi变化至0.8 dBi；天线最大辐射方向在物理结构轴向.基于矢量网络分析仪E8362B的天线特性测量结果与数值计算结果基本一致:工作频率从1 3～1 6GHz变化时,增益从-2.3 dBi变化至1.2 dBi；E面方向图主瓣宽度大于 60°,轴向轴比大于35dB,结果表明设计的天线能够满足L波段高功率微波渊量天线低增益小型化要求.     

Structure-Directing Roles of Organic Molecules in the Formation of Aluminosilicate and Aluminophosphate Molecular Sieves Revealed by 2D 1H DQ-SQ NMR Spectroscopy

Understanding of crystallization mechanisms of molecular sieves is driven by the broad range of usefulness and unique properties they possess. It is still difficult to obtain information related to the crystallization mechanism of molecular sieves, partly because the materials are generally prepared under hydrothermal conditions and the whole reaction happens in the “black box” autoclave. In this work, 2D ¹H DQ-SQ NMR results clearly demonstrate that it is not only the electrostatic interactions between organic structure-directing agents (OSDAs) and the framework, but also the correlation among OSDAs playing the dominant structural directing roles during the crystallization process. Our fundamental understanding of the crystallization mechanism of molecular sieves could be of great value to design and synthesize new molecular sieves with desirable structural properties.