化学衍生-高效液相色谱法测定硫氰酸根阴离子

以α-溴-2,3,4,5,6-五氟甲苯作柱前衍生试剂,经优化衍生和色谱条件,实现了用高效液相色谱法测定硫氰酸根离子。在ODS柱上,用甲醇-水(80:20)作流动相,于254nm检测,得到线性关系良好的工作曲线,最小检测限为4.7ng。分析了吸烟者唾液样品,回收率为93.7％～101.4％。     

Bentone-34/OV-1毛细管柱的研制及其分离性能

自行研制了Bentone-34/OV-1高效石英毛细管气相色谱柱,并利用该柱分别对二甲苯、二氯苯和二氯甲苯异构体3种体系进行分析.在选用的色谱条件下,难分离物质对二甲苯和间二甲苯分离度达3;间二氯苯和对二氯苯分离度达1 3.结果表明该柱具有分离效果好,分析速度快的优点.     

钴(Ⅱ)与5-(5-硝基-2-吡啶偶氮)-2,4-二氨基甲苯络合物吸附波及其应用

钴 (Ⅱ )在NH3·H2O -NH2OH·HCl-5_(5_硝基_2_吡啶偶氮)_2,4_二氨基甲苯体系中有一灵敏的极谱波 ,其峰电位Vp 为 -1.20V(vsSCE) ,钴质量浓度在0.25～25μg/L范围内与峰电流Ip′有良好的线性关系 ,检出限为0.12μg/L;经多种电化学方法证明该波为络合物吸附波 ,其电极过程为不可逆过程 ,电子转移数为2 ,此外还试验了多种离子对峰电流Ip′的影响;所拟方法已用于维生素B12 和模拟样中痕量钴的测定     

Synthesis and Crystal Structure of a 1-D Chain Zinc（Ⅱ） Coordinated Polymer with N-p-Tolysulfonyl-glutamine

A novel coordination polymer {[Zn(ts-gln)(bipy)]3H2O}n (ts-glnH2=N-p-toly-sulfonyl-glutamine,bipy=2,2-bipyridine) has been prepared and structurally characterized by X-ray diffraction method. It crystallizes in orthorhombic,space group P212121 with a=8.2622(5),b=16.6244(10),c=18.2807(10) ,V=2510.9(3) 3,C22H28N4O8SZn,Mr=573.91,Z=4,Dc= 1.518 g/cm3,μ(MoKa)=1.115 mm-1,F(000)=1192,the final R=0.0262 and wR=0.0662 for 5691 independent reflections with Rint=0.0240. The zinc(Ⅱ) atom is coordinated by N(3) and N(4) atoms of a bipy molecule,two carboxylate O(1) and O(2A) and amino N(1) atoms of ts-gln ligands,resulting in a square-pyramidal geometry. The title complex consists of an infinite zigzag chain of zinc(Ⅱ) ions linked by the carboxylate of N-p-tolysulfonyl-glutamine.     

碱金属改性Y分子筛的甲苯氧化甲基化反应性能及基酸碱性质

碱金属改性Ｙ分子筛的甲苯氧化甲基化反应性能及其酸碱性质＊周灵萍李伟苏明李赫口亘陶克毅＊＊（南开大学化学系，天津３０００７１）关键词Ｙ型分子筛，甲苯，甲烷，氧化甲基化，苯乙烯，乙苯，酸性，碱性分类号Ｏ６４３／ＴＱ４２苯乙烯和乙苯是重要的化工原料．以往合...     

二氧化碳—环氧丙烷—甲苯二异氰酸酯的三元共聚

二氧化碳和环氧丙烷(PO)在阴离子配位催化剂,如二乙基锌和等摩尔的水作用下,可接式(1)发生共聚。但产物聚丙撑碳酸酯(PPC)的热稳定性较差。改进途径之一是在反应中引入甲苯二异氰酸酯(TDI)进行三元共聚。本文报导在双金属阴离子配位催化剂PBM存在下合成一种热稳定性优于PPC的聚碳酸酯聚氨酯(PCPU)的研究结果(式2)。     

Preparation and Characterization of Microencapsulated Hexadecane Used for Thermal Energy Storage

Polyurea microcapsules about 2.5μm in diameter containing phase change material for thermal energy storage application were synthesized and characterized by interfacial polycondensation method with toluene-2,4-diisocyanate and ethylenediamine as monomers in an emulsion system. Hexadecane was used as a phase change material and OP, which is nonionic surfactant, and used as an emulsifier. The chemical structure and thermal behavior of the microcapsules were investigated by FTIR and thermal analysis respectively. The results show encapsulated hexadecane has a good potential as a solar energy storage material.     

乙醇和甲苯组成的最低共沸混合物热力学性质的研究

The molar heat capacity of the azeotropic mixture composed of ethanol and toluene was measured by a high precision adiabatic calorimeter from 80 to 320 K. The glass transition and phase transitions of the azeotropic mixture were determined based on the heat capacity measurements. A glass transition at 103.350 K was found. A solid-solid phase transition at 127.282 K, two solid-liquid phase transitions at 153.612 and 160.584 K were observed, which correspond to the transition of metastable crystal to stable crystal of ethanol and the melting of ethanol and toluene, respectively. The thermodynamic functions and the excess ones of the mixture relative to the standard temperature 298.15 K were derived based on the relationships of the thermodynamic functions and the function of the measured heat capacity with respect to temperature.     

Synthesis of Pharmaceutical Intermediates by Toluene Benzylation over Heteropoly Acids on Different Support

Selective formation of pharmaceutical intermediates like diphenylmethane, dimethyl- diphenylmethane, benzyl toluene and benzoic acid by liquid phase, toluene benzylation with benzyl chloride as a benzylating agent, was systematically studied over plane clay (K-10, montmorillonite), plane H-Beta, plane MFI structured titanosilicate (TS-1) and heteropoly acids [HPA, namely dodeca-tungstophosphoric acid [H3PO4.12WO3.xH2O] (TPA), dodeca-molybdo phosphoric acid ammonium salt hydrate [H12Mo12N3O40P aq] (DMAA), sodium tungstate hydrated purified [Na12WO4.2H2O] (STH)] supported on clay, H-beta and TS-1. The 20%TPA/Clay, 30%TPA/H-Beta and 30%TPA/TS-l, were observed to be the best catalyst samples over plane clay, plane H-Beta and plane TS-1. The catalyst samples are compared with respect to benzyl chloride conversion and selectivities for diphenylmethane, dimethyl-diphenylmethane, benzyl toluene and benzoic acid. The reaction follows the pseudo-first order rate power law model. The apparent rate constants are calculated and compared with the reported ones.     

Cu-V-O氧化物催化燃烧甲苯的活性和抗硫性

采用溶胶-凝胶法制备一系列不同Cu/V比例的Cu-V-O催化剂,利用XRD、BET、H₂-TPR等手段对催化剂进行了表征,并考察其催化燃烧甲苯的活性和抗硫性。结果表明,适量的Cu掺杂会提高催化剂比表面积,而且Cu-V可以形成Cu₃V₂O₈晶型结构,使V₂O₅晶格氧活动增加,提高催化剂氧化-还原能力。其中,Cu_0.15V_0.85催化剂表现出最佳的活性和抗硫性;通过TiO₂负载可以进一步提高催化剂对甲苯的催化燃烧活性和抗硫性。