超分子结构二氟尼柳插层镁铝水滑石的合成与表征

采用离子交换和共沉淀两种不同方法将二氟尼柳插入镁铝水滑石层间，得到一种新型的有机-无机层状复合材料。通过X射线粉末衍射、红外光谱、元素分析和热重-差热等手段对材料进行了表征。结果表明，离子交换法和共沉淀法成功地将二氟尼柳插入水滑石，得到的材料层状结构完整、晶相单一，且层间距均大于二氟尼柳分子尺寸，扩大为1.81～2.14 nm；二氟尼柳插入后，复合水滑石材料的热稳定性大幅度提高。客体二氟尼柳与主体层板之间存在超分子作用力，二氟尼柳分子的羧基与水滑石层板之间相互作用，以双层倾斜交替地排列于层板之间。此外，根据其超分子作用力建立了二氟尼柳插层镁铝水滑石的超分子结构模型。     

Effect of pressure on the proton transfer rate from a photoacid to a solvent. 4. Photoacids in methanol

The pressure dependence of the excited-state proton dissociation rate constant of four photoacids, 2-naphthol-6,8-disulfonate (2N68DS), 10-hydroxycamptothecin (10-CPT), 5-cyano-2-naphthol (5CN2), and 5,8-dicyano-2-naphthol (DCN2), are studied in methanol. The results are compared with the results of the pressure dependence study we recently conducted for several photoacids in water, ethanol, and propanol. The pressure dependence is explained using an approximate stepwise two-coordinate proton transfer model. The increase in rate, as a function of pressure, manifests a strong dependence of proton tunneling on the distance which decreases with an increase of pressure between the two oxygen atoms involved in the process. The decrease in the proton transfer rate with increasing pressure reflects the dependence of the reaction on the solvent relaxation rate. We found that, for the relatively weak photoacids 2N68DS, 10-CPT, and 5CN2, the proton transfer rate constant increases by a factor of about 5-8 at a pressure of about 1.5 GPa. For a strong photoacid like DCN2, the rate increase was only by a factor of 2.     

纳米TiO_2改性蚕丝丝素蛋白膜的研究

用溶胶凝胶法制备纳米TiO2改性再生蚕丝丝素蛋白膜.该丝素膜机械强度提高,在水中溶失率下降.UV、AFM、SEM测试的结果表明,丝素中纳米TiO2粒径约为80 nm,纳米粒子在丝素膜中分布均匀;XRD、FTIR测试结果表明,纳米TiO2的加入,可使改性丝素膜的结晶结构从SilkⅠ向SilkⅡ转化,其结晶度也随之提高;TGA测试表明改性丝素膜的热转变温度比纯丝素膜有所改变.     

5-溴水杨基荧光酮-溴化十六烷基三甲基铵吸光光度法测定微量锗

研究了在表面活性剂CTMAB存在下锗与5-溴水杨基荧光酮形成配合物的显色反应,在2mol·L~(-1)H_2SO_4介质中测得配合物的表观摩尔吸光系数为1.62×10~5.锗量在0～8μg/25ml范围内符合比耳定律.该体系反应酸度高,选择性好.方法稳定、决速.已用于水相直接测定人参、当归、灵芝、枸杞子和竹沥汁等中药材中微量锗,结果满意     

高锰酸钾法、碘量法和铈量法测定过氧化氢的比较

过氧化氢是一种常用的化学试剂，可作为消毒剂、杀菌剂、脱氧剂、漂白剂和聚合反应的引发剂等。目前过氧化氢的分析方法有高效液相色谱法、紫外分光光度法、流动注射-分光光度法和化学滴定法、高锰酸钾法、碘量法和硫酸铈法等。本文分别对高锰酸钾法、碘量法和铈量法测定过氧化氢进行比较。     

Double cyclisation of phenylglycine-o-carboxylic acids—I: New stable mesoionic oxazolones

Remarkably stable mesoionic oxazolones possessing an oxazolo[3,2-a]quinolinium structure (5a–b),8,16, 17) were obtained by the double cyclisation of phenylglycine-o-carboxylic acids (3a–c) in refluxing acetic anhydride or in benzoic anhydride at 140°, The 0-Ac group was eliminated to give the corresponding lactones (6a–b) or replaced by O-Ts (7). IR stretching vibrations of the endo-carbonyl were in the range 1710–1768 cm^?1, while v_1-CH exhibited unusually high values (3159–3194 cm^-1). 1-Acyl derivatives could be obtained only with TFAA (23–24), although easy deuteration of the same position took place in the presence of traces of trifluoroacetic acid. Hydrolysis of 5b led to the α-quinolone-N-acetic acid 27a. In the case of 5a, hydrolysis was accompanied by self-acylation of the nucleophilic site at C-4 with formation of a dimeric acid 28a. The presence of an additional Me group in phenylalanine-o-carboxylic acid (36) activates the corresponding mesoionic oxazolone 37 so that 1-acylation becomes possible with formation of the fused oxazole 38 by the Dakin-West reaction. Temperature dependent magnetic non-equivalence of methylene protons has been observed in acids 3b-d and f and also in the 7-membered anhydride 48b.     

超高交联吸附树脂对芳香有机物的吸附机理

通过3种吸附树脂AmberliteXAD-4、AM-1和JX101对芳香化合物苯胺、苯酚和苯甲酸在不同温度下的吸附特征,利用前线轨道理论进行了合理解释。结果表明,吸附剂表面进行适当的修饰,可以改变吸附剂的LUMO或HOMO,使吸附质分子与吸附剂表面的功能基产生化学作用,从而产生额外的化学吸附量,为优化设计吸附剂提供了理论指导。     

PMR-Spektren einiger Alkoxy-9-chlor-6-nitroacridine

The spectra of some 9-chloro-6-nitroacridines with methoxy substituents in position 1,4; 2,4; 3,4; 2,3; and ethoxy substituents in positions 1, 2, 3, were recorded. The influence of electron releasing alkoxy groups and electron withdrawing nitro groups on chemical shifts of protons in the 9-chloroacridinic cycle was discussed and PMR parameters were determined, comparatively with those of acridine and 9-chloroacridine. Good agreement between calculated and experimental values is observed. The spectrum of 9-chloro-1,2,3-triethoxyacridine shows for the four protons of the ringC. (H-5, H-6, H-7, H-8) anAMNX coupling pattern whose parameters were determined.     

一种高灵敏的压电免疫传感器用于高密度脂蛋白的测定

采用自组装单层膜(SAMs)技术在压电石英晶体的金电极表面组装巯基丙酸SAMs,以盐酸1-乙基-3-(3-二甲基氨基丙基)碳二亚胺(EDC)和N-羟基琥珀酰亚胺(NHS)作偶联剂,以共价键合方式固定高密度脂蛋白抗体,研制成一种高灵敏的压电免疫传感器用于检测人血清中低含量的高密度脂蛋白。利用压电装置的实时监测功能,考察了巯基丙酸在金电极表面的自组装成膜过程与机制;研究了晶振固定抗体及其反应结合抗原的液相振荡行为和传感特性。传感器采用初始速率法测定高密度脂蛋白的线性浓度范围为1.63~18.8 mg.L-1,检出限为0.82 mg.L-1。     

超高交联树脂对苯胺的吸附机理研究

在静态条件下，研究了水溶液中超高交联树脂AM－1和NJ－8及大孔吸附树脂Amberlite XAD－4吸附苯胺的热力学特性，测定了不同温度下的吸附等温线。结果表明，在稀溶液中3种树脂吸附苯胺都符合Langmuir和Freundlich模型，其中AM－1和NJ－8对苯胺的吸附是一个吸热过程；由于AM－1和NJ－8的微孔结构和表面存在酸性基团的吸附中心，对苯胺的吸附是物理吸附和化学吸附共同作用的结果。