端视等离子体原子发射光谱仪的性能评价

端视等离子体原子发射光谱仪与侧视等离子体原子发射光谱仪相比在分析性能方面所表现出来的差异一直是光谱分析工作者所关注的一个重要方面。此文较系统的总结了近年来在此方面所做的研究工作，引用47篇文献。     

高效液相色谱法拆分雷喏嗪

用高效液相色谱法(HPLC)在正相条件下,用自制的涂敷直链淀粉-三(3,5-基苯基氨基甲酸酯)(ADMPC)手性固定相直接拆分了高效低毒的抗心绞痛药物雷喏嗪外消旋体(Ranolazine),并考察了二元及三元流动相体系对样品分离的影响,结果表明,三元流动相中的拆分结果远远好于二元流动相,流动相中不同种类醇改性剂及含量对样品保留时间和立体选择性有不同程度的影响．     

基于差示扫描量热技术的生物质热解两步连续反应模型研究

采用差示扫描量热分析仪对我国的一种生物质试样在空气气氛中进行了实验, 发现试样从常温到923 K高温的低速升温过程中, 经历了两步明显的放热过程. 对放热机理的分析表明, 第一步主要是由半纤维素和纤维素的有氧热解过程控制, 第二步放热过程则受木质素热解和炭的氧化反应的共同作用. 采用等转化率方法和优化计算方法, 对热解过程的动力学模型进行了研究, 结果表明, 两步连续反应机理可用于描述生物质在空气气氛中热解的放热动力学.     

稀土铜硫化合物TbCuS2的合成和晶体结构

Terbium copper disulfide, TbCuS₂, has been synthesized in the reaction of the elements in a KI flux at 850 ℃. The compound crystallizes in space group P2₁/c of the monoclinic system with four formula units in a cell of dimensions of a= 0.639 3(1) nm, b=0.702 5(1) nm, c=0.670 8(1) nm, β=98.097(4)°, and V=0.298 3(1) nm³ at 153 K. The structure comprises two-dimensional ²_∞[CuS₂] layers along [100] separated by the Tb atoms. In the structure, each Tb and Cu atoms are coordinated to seven and four S atoms, respectively. CSD: 415490.     

三维银配位聚合物[Ag3(IN)2(CF3COO)]的水热合成与晶体结构

本文在水热条件下, 通过4-氰基吡啶发生原位水解得到异烟酸, 将其与AgCF3CO2作用合成了新型银配位聚合物, 并通过元素分析和X射线单晶衍射分析等手段对其结构进行了表征.     

芳酸及其衍生物的三氯甲基化反应的研究

首次报道了以四氯苯膦为转化剂或采用二氯苯膦与五氯化磷相结合, 将芳酸或芳酰氯转化为三氯甲基芳烃. 同时, 对影响反应的因素进行了研究, 发现连有推电子基的二氯苯膦有促进反应的作用, 而连有吸电子基团则减缓反应的进行, 而反应底物(芳酸或芳酰氯)的结构效应则相反: 连有吸电子基的芳酸有利于反应, 而连有推电子基团则减缓反应的进行. 此外, 发现反应中生成的苯膦酰二氯可作为催化剂重复使用, 并对转化反应的条件进行了改进与优化, 合成出9个三氯甲基芳烃, 其中2个是未见文献报道的新化合物.     

四羧基金属酞菁负载纤维素纤维的制备及其消臭性能研究

合成了四羧基铁酞菁(Fe-CPc)和四羧基钴酞菁(Co-CPc),并对其进行了元素分析和红外光谱表征.在酸性条件下,将四羧基金属酞菁负载到改性纤维素纤维上,制备得到消臭纤维.实验结果表明,在室温条件下,四羧基铁酞菁消臭纤维(FePcF)、四羧基钴酞菁消臭纤维(CoPcF)和混合金属酞菁消臭纤维(CoFePcF)3种功能性纤维都能有效去除甲硫醇、硫化氢、氨气和三甲胺,甲硫醇和硫化氢按催化氧化机理除去,而氨气和三甲胺按酸碱中和机理除去;3种消臭纤维对甲硫醇和硫化氢的消臭效果为CoFePcF>CoPcF>FePcF.     

An Efficient Deselenenylation Reaction to the Synthesis of 3, 5-Disubstituted Isoxazoline and Isoxazole

The development of organoselenium chemistry1 has been expanding rapidly during the last decades. Among them, organic selenides are key intermediates, for that they can be efficiently introduced, manipulated, and removed through selenoxide syn-elimination2. Our research group3 has been interested in the application of selenium in organic synthesis for several years. Isoxazolinyl substituted phenyl selenide 13a, although a β-H exists in the molecule, did not undergo selenoxide syn-elimination e…     

SYNTHESIS OF FUNCTIONAL MACROMOLECULE INTERMEDIATE THROUGH ACYLATION CATALYZED BY [Emim]Cl-AlCl3 IONIC LIQUID

Acylation reaction of anthracene with oxalyl chloride in the presence of [Emim]Cl-AlCl3 ionic liquid has been investigated. Pure 1,2-aceanthryenedione, which is used as intermediate of functional aromatic polymer material, was obtained by recrystalling the reaction mixture with aether and was determined by GC/MS, 1↑HNMR and FTIR analysis. The influences of various parameters, such as the contents of AlCl3 in [Emim]Cl-AlCl3, the amount of acylation agent, amount of [Emim]Cl-AlCl3, reaction temperature and reaction time were investigated. The optimum conditions were as follows： the molar fraction of AlCl3 in ionic liquid [x（AlCl3）] being 0.67, molar ratio of ionic liquid to anthracene being 2：1, molar ratio of oxalyl chloride to anthracene being 2：1, reaction temperature being 40℃ and reaction time being 6h. Under above conditions, the yield and selectivity of 1,2-aceanthrylenedione can reach 91.5% and 98.3% respectively. Further more, [Emim]Cl-AlCl3 ionic liquid, compared with metal halides such as AlCl3, was found to catalyze the reaction as a novel environmental friendly catalyst and solvent and can be reused.     

二维配位聚合物[K2(5-nbdc)2Cd(Ⅱ)·imH·H2O]∞的合成和晶体结构(英)

The crystal structure of the title complex, [K₂(5-nbdc)₂Cd(Ⅱ)·imH·H₂O]_∞ (5-nbdc=5-nitro-1,3-benzenedicarbonate, imH=imidazole) has been determined by X-ray diffraction analysis. The crystal data are: tetragonal, space group P4₁, M_r=694.93 for CdC₁₉H₁₂N₄O₁₃K₂, a=1.018 6(10) nm, b=1.018 6(10) nm, c=2.436 7(5) nm; Z=4, V=2.528 2(6) nm³, F(000)=1 376, D_c=1.826 Mg·m^-3, μ=1.267 mm^-1. The title polymeric complex exhibits a two-dimensional framework, in which adjacent Cd(Ⅱ) ions are bridged by μ-O₄-5-nitro-1,3-benzenedicarbonate groups forming one-dimensional chains that are further linked by μ-O₃-5-nitro-1,3-benzenedicarbonate groups into two-dimensional anion rectangle sheets with large 32-membered rings. The strong π-π stacks of the benzene rings link these adjacent sheets into a three-dimensional van der Waals network. CCDC: 245527.