锕系多重键金属有机化合物研究进展

多重键金属有机化合物在多种催化反应中已经得到广泛的应用, 并取得了很好的研究成果. 目前, 多重键金属有机化合物的研究已成为催化化学领域中一个引人注目的研究热点. 综述了锕系多重键金属有机化合物的研究进展. 根据化合物多重键的不同, 分别讨论了它们的合成及反应性能, 并定性讨论了多重键的性质.     

Coupling of thermal desorption in modified closeable sampling columns with wide-bore capillary gas chromatography and mass spectrometric detection

In contrast to usability of Curie-point pyrolysis at 700°C directly attached to gas chromatography-mass spectrometry (GC-MS) for determination of organic wood preservatives in waste wood samples the investigation method reported here consists of thermal desorption at temperatures about 260°C in connection with GC-MS for peak identification or GC with flame ionization detection for quantitative analyses. So-called “modified closeable sampling columns” are used as batch-reactor in thermal desorption experiments. Desorbed vapours can be introduced on capillary columns without sample discrimination and without a disturbing lost of resolution. In this manner a lot of individual polycyclic aromatic hydrocarbons were determinated in waste wood samples, especially in railway sleepers.     

Glass capillary gas chromatography of amino acid enantiomers

Glass capillaries coated with Chirasil-Val, a chirally functionalised polysiloxane, are capable in principle of resolving all protein amino-acid enantiomers in a single run and within a short analysis time, thus allowing for example the quantitative amino acid determination by enantiomer labelling. The elution characteristics of the individual amino acids however are also dependent upon the chemical nature of the capillary wall surface, and a surface pretreatment is found to be necessary if all protein amino acids are to be analysed. Of the various methods of pretreatment tested, etching of borosilicate glass with gaseous HCl followed by deposition of colloidal silicic acid is considered to be the most suitable.     

酰胺型萃取剂N-503的合成

酰胺型萃取剂N-503[N,N-二-(1-甲基庚基)乙酰胺]可以用甲庚醇或2-氯代辛烷为原料来合成。它的重要中间体二-(1-甲基庚基)胺的制备方法有二:一是从甲庚醇制备的方法,将甲庚醇用阮来镍催化,常压氨解,得率95～99％左右;二是从2-氯代辛烷制备,此法需要高压设备,得率35％左右。第一个方法在扩大试验中,产率和产品质量都比较好,是一个较好的制备长碳链仲胺的方法。     

Darstellung und Kristallstruktur von LnAl3Br12 (Ln = La,Ce, Pr,Nd, Sm,Gd) und thermischer Abbau zu LnBr3

Preparation and Crystal Structure of LnAl₃Br₁₂ (Ln = La, Ce, Pr, Nd, Sm, Gd) and Thermal Decomposition to LnBr₃ LnAl₃Br₁₂ (Ln = La, Ce, Pr, Nd, Sm, Gd) was prepared in crystalline form for the first time. The crystal structures of LaAl₃Br₁₂, PrAl₃Br₁₂, and NdAl₃Br₁₂ were determined on single crystals by X-ray methods. The isotypic compounds crystallize with trigonal symmetry, space group P 3₁12, Z = 3. A structural comparison to lanthanoide chloroaluminates of equal composition is given and thermal decomposition of LnAl₃Br₁₂ (Ln = Nd) to the corresponding lanthanoide tribromide is described.     

葡萄糖氧化酶电极的制备

葡萄糖氧化酶电极的制备于秀娟，周定，郭京华（哈尔滨工业大学应用化学系哈尔滨１５０００６）关键词葡萄糖氢化酶，酶电极，制备酶与电极的连接即酶膜的形成是制备酶电极的关键步骤之一，有许多种方式［１～９］．葡萄糖氧化酶（ＧＯＤ）电极是研究较早和报道较多的一类...     

硝酸钆低水合物的制备及表征

本文用两种方法制得硝酸钆的低水合物Gd(NO_3)_3·5H_2O、Gd(NO_3)_3·3.5H_2O,其中Gd(NO_3)_3·3.5H_2O是文献中尚未报道的 ,给出了它们的M.P.和X-衍射特征值。     

一锅法制备全乙酰吡喃溴代糖

将未保护的吡喃糖与醋酸酐在分子碘的催化下制得全乙酰吡喃糖 ,随后不经分离直接与溴化氢的冰醋酸溶液( 4 5 %)反应得到全乙酰吡喃溴代糖 .这种一锅法制备全乙酰吡喃溴代糖操作方便 ,收率高 ,经济实用且对环境友好     

高效除草剂快杀稗标准物质的制备及表征

从快杀稗工业品出发 ,经活性炭纯化、硅胶柱层析分离制得快杀稗标准物质 ,并进行熔点、高效液相色谱、紫外光谱、元素分析、红外光谱、质谱、核磁共振等方法的表征 ,以高效液相色谱法测得该标准品纯度在99%以上     

氨基硫脲及其相关化合物的化学

本文综述了氨基硫脲及其相关化合的合成、波谱和化学性质以及在药物、工业、农业等方面的应用。