一种西佛碱侧链型液晶高分子的合成及表征

一种西佛碱侧链型液晶高分子的合成及表征邹友思，林国良，姚青青，戴李宗，潘容华（厦门大学化学系厦门３６１００５）关键词联苯，西佛碱，侧链型，液晶高分子，基团转移聚合Ｆｉｎｋｅｌｌｎａｎｎ等提出的柔性基去偶合概念’］已在侧链型液晶高分子的研究中得到了证实...     

Study on the Chromatographic Behavior of Bases on Dodecylamine-N,N-dimethylenephosphonic Acid-Modified Zirconia Stationary Phase

A new zirconia-based stationary phase (DPZ) was prepared by modifying zirconia with dodecylamine-N,N-dimethylenephosphonic acid (DDPA). DDPA was adsorbed on zirconia with only one phosphonic group, with the other being free. Besides the hydrophobic interaction provided by nonpolar dodecyl, DPZ also has dipolar interaction, ion-exchange or electrostatic repellent interaction provided by the free phosphonic group and amino group at different conditions. Separation of bases on this stationary phase was achieved with satisfaction owing to the various retention mechanisms. The influence of methanol content, pH value, ion types, and ionic strength of mobile phase are studied in detail. Translated from Chinese Journal of Chromatography, 2005, 23(1) (in Chinese)     

含硫希夫碱的合成研究

合成了一种含硫希夫碱—1，4-双[(2’-甲醛缩硫代氨基脲基)苯氧甲基]乙烷及其中间产物1，4-双[(2’-甲醛)苯氧甲基]乙烷．其结构经元素分析，IR和1H NMR表征。     

过渡金属离子与Schiff碱配合物的研究——Ⅰ.双-[N-(4-甲基苯基)水杨醛亚胺]钴(Ⅱ)的晶体结构与电子结构

过渡金属离子与Schiff碱配合物的合成与性质研究始自50年代,并已有不少论文发表。70年代发现Co(Ⅱ)与Schiff碱的配合物具有抗癌和抗肿瘤活性之后,这一领域的研究工作更加活跃,但对其结构和性质关系的研究多数尚通过谱学方法进行,对标题化合物也只有晶胞参数的报导。为了探讨该类化合物的分子结构与生理活性的关系,本文首先报导标题化合物的晶体与分子结构以及其电子结构的量子化学近似计算结果。     

双环[2，2，1]庚-5-烯-2-甲酰基芳香醛腙的合成和生物活性

合成了七个未见文献报道的双环[2，2，1]庚-5-烯-2-甲酰基芳香醛腙席夫碱 类化合物。用核磁共振氢谱、红外光谱和元素分析对新化合物进行了表征，考察了 它们的生物活性。结果表明某些化合物具有除草作用、抗菌作用和植物生长调节作 用。     

Synthesis and Magnetic Properties of Binuclear Mn（Ⅱ）Complexes with Alkoxide Bridge

ＳｙｎｔｈｅｓｉｓａｎｄＭａｇｎｅｔｉｃＰｒｏｐｅｒｔｉｅｓｏｆＢｉｎｕｃｌｅａｒＭｎ（Ⅱ）ＣｏｍｐｌｅｘｅｓｗｉｔｈＡｌｋｏｘｉｄｅＢｒｉｄｇｅＹａｎＳｈｉ－ｐｉｎｇ；ＦａｎＢｏ；ＬｉａｏＤａｉ－ｚｈｅｎｇ；ＪｉａｎｇＺｏｎｇ－ｈｕｉａｎｄＷａｎｇ...     

西佛碱大环双核钴（Ⅱ）配合物的合成,光谱及磁性

本文以２．６─二乙酰吡啶和１，３一二氨基一２一丙醇通过模板合成西佛碱大环配体Ｈ＿２Ｌ（图１），并合成了它的Ｃｏ（Ⅱ）、Ｎｉ（Ⅱ）及Ｆｅ（Ⅱ）的双核配合物，重点讨论了Ｃｏ＿２（ＨＬ）（ＣｌＯ＿４）＿２（ＮＯ＿３）·４Ｈ＿２Ｏ配合物的光谱与磁性。变温磁化率数据（４─３００Ｋ）通过用最小二乘法与理论方程拟合，得到磁参数为Ｊ＝－１．２４ｃｍ￣（－１），θ＝－０．２４Ｋ，表明配合物中ｃｏ（Ⅱ）－Ｃｏ（Ⅱ）间存在弱的反铁磁相互作用，分子间也存在反铁磁相互作用。     

Synthesis,Reactivity, and Structural Characterization of Dioxovanadium(V) Complexes with Tridentate Schiff Base Ligand: Vanadium Complexes in Supramolecular Networks

The synthesis, characterization and crystal structure analysis of the ammonium salt of the dioxovanadium(V) complex NH₄[VO₂(salhyph)] with the tridentate Schiff base ligand derived from salicylaldehyde and benzoic acid hydrazide (H₂salhyph) is reported. NH₄[VO₂(salhyph)] crystallizes in the monoclinic space group Pn with a = 708.8(2), b = 1444.3(3), c = 717.1(2) pm and β = 101.09(2)°. The vanadium atom of the dioxovanadium(V) moiety has a distorted square‐pyramidal coordination geometry. Extensive hydrogen bonding is observed between the ammonium cation and the oxygen atoms coordinated to the vanadium atom yielding to a two‐dimensional network, where the complex anions are arranged in a bilayer. Additional crystal packing within the bilayer appears to be controlled mostly by π stacking between the aromatic rings of the ligand. The reactions of NH₄[VO₂(salhyph)] with several proton acidic compounds including water, methanol, and proton acids lead to neutral monooxovanadium(V) and dioxovanadium(V) complexes ([VO₂(Hsalhyph)], [V₂O₃(salhyph)₂] and [VO(OMe)(salhyph)(HOMe)]).     

化学计量及其进展

扼要介绍了化学计量主要研究内容和量传方法。并从化学计量技术机构,基准、标准装置,标准物质,检定规程和化学计量学等方面,叙述了化学计量的进展概况。     

氢化物发生石墨炉原位富集直接测定高温镍基合金中碲

通过选择碲的氢化物发生条件，克服了高含量镍对碲的干扰，把氢化物富集在涂钯石墨管里，然后再原子化，成功地测定了高温镍基合金中碲。