Syntheses,crystal structures and blue emission of three zinc(II) coordination polymers with a 4,4′‐dicarboxybiphenyl sulfone ligand

Three novel zinc complexes [Zn(dbsf)(H₂O)₂] ( 1 ), [Zn(dbsf)(2,2′‐bpy)(H₂O)]·(i‐C₃H₇OH) ( 2 ) and [Zn(dbsf)(DMF)] ( 3 ) (H₂dbsf = 4,4′‐dicarboxybiphenyl sulfone, 2,2′‐bpy = 2,2′‐bipyridine, i‐C₃H₇OH = iso‐propanol, DMF = N,N‐dimethylformamide) were first obtained and characterized by single crystal X‐ray crystallography. Although the results show that all the complexes 1–3 have one‐dimensional chains formed via coordination bonds, unique three‐dimensional supramolecular structures are formed due to different coordination modes and configuration of the dbsf^2? ligand, hydrogen bonds and π–π interactions. Iso‐propanol molecules are in open channels of 2 while larger empty channels are formed in 3 . As compared with emission band of the free H₂dbsf ligand, emission peaks of the complexes 1–3 are red‐shifted, and they show blue emission, which originates from enlarging conjugation upon coordination. Copyright © 2006 John Wiley & Sons, Ltd.     

氯离子柱撑水滑石共沉淀法合成反应动力学

根据氯离子型层状复合氢氧化物(LDH-Cl)制备过程中溶液浓度变化的监测结果和不同反应进程时产物的EDS、IR、XRD、TEM、TG-DTA表征结果,研究了合成LDH-Cl的共沉淀反应动力学特征及机理.实验结果表明, LDH-Cl的生成符合多核层表面反应动力学模型;反应过程中LDH的晶胞参数c从2.421 nm变为2.399 nm,通道高度h由0.3321 nm减小为0.3228 nm,粒子直径Da由6.40 nm增大为15.16 nm, Dc由7.43 nm增大到10.93 nm,纵横比由0.86增大为1.39; IR和TG-DTA特征变化表明了层板对阴离子作用的强度和层板的结构稳定性随反应进程而提高.     

毛细管凝胶电泳的激光光热在线检测

近年来,毛细管电泳已成为一种高效快速的微化学分离分析新技术,在无机、有机及生物化学分析中得到了广泛的应用.但毛细管的内径小,进样量在pg～ng级,给样品的检测带来新的困难.因此,发展高灵敏度的显微在线检测器,已成为毛细管电泳技术发展中的重要环节.基于各种原理的检测器研究已有报道~[1].Dovichi等曾用热透镜技术在线检测了乙腈/     

Synthesis,crystal structure and property of a novel azide-bridged one-dimensional chain copper(II) complex with a dinucleating macrocyclic polyamine

An azide-bridged polymeric cationic chain complex, [LCu₂(N₃)₂]n(ClO₄)_2n ·n(H₂O)**, where L=the dinucleating macrocyclic ligand bis-p-xylylBISDIEN, has been prepared and characterized by x-ray crystallography, u.v.-vis and i.r. spectra, and by magnetic measurements. The structure consists of cationic azide-bridged [LCu₂(N₃)₂]²⁺ (unit) chains, non-coordinated perchlorate anions and crystallized water molecules. The azide anion is bound to two copper atoms in neighboring units with an end-to-end bridging mode. In each unit, the copper atoms have a different coordination geometry; Cu(1) is a four-coordinated, distorted square-planar geometry, whereas Cu(2) is a five-coordinated, distorted square-pyramid. The electronic spectra of the title complex differ in anhydrous and in aqueous MeCN solutions, indicating that dissociation and solvation occur in aqueous solutions. The characteristic i.r. absorptions of azides and perchlorates are described. Magnetic moments vary from 2.05 (B.M.) at 300K to2.01 (B.M.) at 80K, which suggests that very weak interactions exist between the metals.     

高纯度植酸的制备

高纯度植酸的制备孙定光胡佩廖显威（四川师范大学化学系成都６１００６６）关键词植酸制备高纯试剂中图分类号Ｏ６２９．９植酸（ＰｈｙｔｉｃＡｃｉｄ）又名肌醇六磷酸酯，分子式：Ｃ６Ｈ１８Ｏ２４Ｐ６，结构为植酸是中等强度的有机酸，因其结构特殊，具极强的螯合作用...     

测接触角法确定偶联剂的最佳用量

偶联剂是一类能在无机填料和聚合物基材之间形成“分子桥”、改善两者之间相容性或提高两者之间相互作用能力的化合物。将经偶联剂改性的无机填料填充到聚合物中可以制得成本低、性能好的复合材料。由于偶联剂用量多少将对复合材料的性能产生较大影响,因此建立一种准确、简便地确定偶联剂最佳用量的方法有着十分重要的理论和实际应用意义。     

少量人发中硫的测定

建立了测定一根长2～3cm人发中硫的间接分光光度法,表观吸光系数为5.1×10~4,络合物组成Ba:CPA-mA为1:2,比耳定律范围为0～20μg硫。硫的检测限为0.025μg/mL,变动系数为2.7%,回收率为91.2～97.2%,且不用掩蔽即可直接进行测定,测定211例人发的结果表明,含硫量范围为(28.5±3.2)×10~3μg/g。     

含液晶基团的聚对亚苯基亚乙炔基类交替共聚物的合成、表征及性能研究

合成了两种含氰基联苯液晶基团的新型聚对亚苯基亚乙炔基(PPE)类交替共聚物,并对其进行了结构表征和性能研究.示差扫描量热仪(DSC)和偏光显微镜(POM)的结果证明了在液晶单元含量较大时聚合物才会出现明显的液晶形态.荧光光谱表明,在降温前后液晶聚合物的发光光谱发生了明显的变化.同时,对聚合物进行能量转移研究发现随着溶液浓度的增加,Frster能量转移更加完全;另外,利用原子力显微镜(AFM)对聚合物降温前后的形态变化进行了观察.结果表明,液晶性质可以导致聚合物形态的变化进而带来发光光谱的改变,为今后制备液晶可控型发光聚合物提供了理论依据.