组合脱胺对β沸石酸性和结构的影响

利用ＴＰＤＥ、ＴＰＤ和ＸＲＤ等手段研究了低温恒温脱胺后再程序升温脱胺的组合脱胺法．结果表明，不同组合脱胺工艺均可调变β沸石的表面酸性，适当选择组合脱胺温度可大幅度调变β沸石的表面酸性，其中２７０℃和２９０℃下分别恒温脱胺后再程序升温脱胺，β沸石表面除出现传统脱胺的两个酸性位外，还出现了一个中等强度的酸性位，且酸量很大，可调变性较强．晶相测定可知，低温脱胺后再程序升温脱胺有利于β沸石结晶度的保持．此外，还对β沸石的脱胺过程和脱胺后β沸石的吡啶脱附过程的动力学行为进行了初步的研究．     

组合脱胺对β沸石酸性和结构的影响

利用ＴＰＤＥＴＰＤ和ＸＲＤ等手段研究了低温恒温脱胺后的再程序升温脱胺的组合脱胺法，结果表明，不同组合脱胺工艺均可调度β沸石的表面酸性，适当选择组合脱胺温度可大幅度调度β沸石的表面酸性，其中２７０℃和２９０℃下分别恒温脱胺后程序升温脱胺，β沸石表面除出现传统脱胺的两个酸性位外，还出现了一个中等强度的酸性位，且酸量很大，可调变性较强，晶相测定可知，低温脱后再程序升温脱妥有利于β沸石结晶度的保持，此外，     

人尿中多胺的离子交换富集和气相色谱测定

以离子交换法对尿样中的多胺进行预分离富集，确定了最佳的离子交换条件，同时比较了三种不同酰化剂的酰化效果，确定了最佳酰化条件，并用毛细管气相色谱法测定了尿中腐胺，尸胺，精脒，精胺的含量，结果表明癌症病人尿中多胺含量高于正常人。     

合成丙二酸亚异丙酯Mannich碱的新方法

以甲醛和胺作为胺甲基化试剂，合成了丙二酸亚异丙酯及其5－单取代烃基衍 生物的Mannich碱，同时还讨论了这些Mannich碱的化学性质。     

不同有机胺对合成杂原子Ga－Si－ZSM－5分子筛的影响

考察了几种有机胺作引导剂对以水玻璃为硅源、硝酸镓为镓源合成Ｇａ－Ｓｉ－ＺＳＭ－５分子筛的影响。结果表明，合成体系的最佳碱度与有机胺有关，不同有机胺的合成效果相差很大，以正丁胺作引导剂可获得高结晶度的分子筛产物。通过与合成Ａｌ－Ｓｉ－ＺＳＭ－５的比较和一些条件试验，探讨了有机胺的作用，并对分子筛的形成过程进行了合理的推测。     

炔基苯甲酰胺衍生物的液相合成

液相合成兼容了固相合成可快速简便地对产物进行分离纯化以及溶液相合成可 在均相条件下进行反应和用常规手段对反应中间体进行分析检测的优点，用聚乙二 醇(PEG)4000作为可溶性聚合物支持体，通过醚键将[1，3，5]氯三嗪连接在PEG上 制备成PEG支持的新型的可溶性聚合物试剂I．该试剂在N-甲基吗啉的作用下与对碘 苯甲酸反应生成相应的活性酯中间体Ⅱ，该中间体继而在Pd(Ⅱ)／Cu(Ⅰ)共催化下 与端炔发生Sonogashira偶联反应得到另一中间体Ⅲ，在伯胺或仲胺的存在下进行 胺解反应得到炔基苯甲酰胺衍生物Ⅳ．由于PEG具有柔韧的长链而不会对链端连接 的反应中心的活性产生影响，因此该反应在均相体系中进行，不仅反应条件温和， 产率良好，而且反应还具有良好的选择性．实验发现，芳香胺和非芳香胺均可获得 良好的反应结果，但芳香胺所需的反应时间较长；伯胺和仲胺都是良好的胺解试剂 ，但使用仲胺时产率较低；N原子亲核试剂比O原子亲核试剂具有更大的反应性．此 外，PEG 4000支持的[1，3，5]氯三嗪试剂没有强烈的刺激性，可长期储存使用．     

耐高温梯形聚甲基倍半硅氧烷的合成研究

以有机伯胺为胺解剂，与甲基三氯硅烷反应形成梯形结构的“模板”，经水解，缩聚反应，合成了梯形聚甲基倍半硅氧烷，研究了水解温度，溶剂，水与单体的摩尔比，缩聚温度，缩聚时间以及胺的结构对产物性能的影响，获得了最佳的合成条件，产物经热重分析，表明其耐热性能优良，７００℃失重率仅为４％。     

双胺醚制备中二乙烯三胺和双胺醚的气相色谱分析

双胺醚制备中二乙烯三胺和双胺醚的气相色谱分析张惠良，施耀增，杜争鸣，吕槊贤，阮劲松（南京大学化学系，南京，２１０００８）关键词：双胺醚；二乙烯三胺；气相色谱分析ＣＨ＿３＼双胺醚［Ｎ—ＣＨ＿２—ＣＨ＿２］，亦称双（Ｎ，Ｎ－二甲胺基乙基）醚，可采用二乙烯...     

C_（60）与含烯丙基胺聚合物加成物的荧光行为

Ｃ_（６０）与含烯丙基胺聚合物加成物的荧光行为田慧洁，陈立桅，姚光庆，金朝霞，李福绵（北京大学化学系北京１００８７１）关键词脂肪胺，Ｃ_（６０），聚烯丙基胺，荧光Ｃ６０是一高度对称的笼状碳簇分子，室温下难以观察到荧光现象［１］，但我们发现它与聚烯丙基胺...     

全固态竹林胺传感器的研制和应用

全固态竹林胺传感器的研制和应用李荣华，乔宏斌（河南教育学院，郑州４５０００３）１引言竹林胺为ａ－肾上腺素受体阻滞药，现行分析标准为非水滴定法，不适于含碱性杂质的样品，而且手续繁复。本文首次报道了聚苯胺修饰竹林胺传感器的研制和应用。将具有较高导电性、良...     

南瓜籽烘烤前后化学成分的分析

对烘烤前后南瓜籽中的化学成分进行分析并对比。采用同时蒸馏萃取装置萃取南瓜籽中的挥发性成分,采取超临界CO2萃取技术萃取南瓜籽油脂,并将其分为酸、碱、中性三个部分,用气相色谱-质谱联用方法分析其中化学成分并进行对比。结果表明,南瓜籽挥发性成分中含有多种醛类和酯类化合物,烘烤后产生了大量的烷基吡嗪,其在碱性部分中的相对含量比烘烤前提高14倍多,不饱和醛类化合物含量也有明显提高。南瓜籽油脂中的主要化学成分是油酸、亚油酸及其酯类。还含有生物活性功能成分如植物甾醇、角鲨烯和维生素E等。烘烤后除角鲨烯含量有所降低,维生素E、植物甾醇、亚麻酸等均有提高。     

Preparation and properties of polyurethane networks based on α,ω-difunctional poly(hexafluoropropylene oxide)

Poly(hexafluoropropylene oxide), poly(HFPO), networks were prepared from functional polymers by end linking via urethane groups. The prepolymers were characterized by NMR spectroscopy and GPC. The networks were characterized by determination of the number of network chains from the shear modulus, and were snown to contain both trifunctional crosslinks and difunctional links. The properties of the networks were investigated by a range of techniques. Compared with fully-fluorinated networks formed via triazine cross-links, investigated previously, the urethane-linked networks were more readily prepared but were poorer elastomers, were less thermally stable, and were less resistant to swelling by common polar solvents. © 1995 John Wiley & Sons, Inc.     

云南菊科中草药中铅含量特征分析

论述了云南２７种菊科中草药及其水提取物中铅含量的特征。菊科植物及水提物中铅含量的频数分布为正偏态,两者的相关系数ｒ＝０．０９,未呈现显著的线性相关。提取率较高的山紫苑、佩兰、木香铅实际含量低;铅含量高的叶下花、狭叶兔耳风、臭灵丹提取率又较低,减少了人体对Ｐｂ的过量摄入。     

碳苷研究 V: 用Grignard试剂合成取代苯酚中酚羟基的保护及脱保护

本文报道了一些取代苯酚的合成, 并探讨了用Grignard试剂合成取代苯酚中酚羟基的保护及脱保护的问题. 利用苄基和甲基作为酚羟基的保护基, 对文献报道的切断醚键脱保护方法进行了评价. 找到了两种新体系能在更温和条件下切断醚键的方法, 指出了它们的适用条件. 实验结果符合硬软酸碱理论.     

FT-IR, FT-Raman spectra, density functional computations of the vibrational spectra and molecular geometry of biomolecule 5-aminouracil

FT-IR and FT-Raman spectra of the biomolecule 5-aminouracil were recorded in the regions 400–4000 cm⁻¹ and 10–3500 cm⁻¹, respectively. The observed vibrational wavenumbers were analyzed and assigned to different normal modes of vibration of the molecule. Density functional calculations were performed to support wavenumber assignments of the observed bands. A comparison with the molecule of uracil was made, and specific scale factors were employed in the predicted wavenumbers of 5-aminouracil. With the purpose of study the important molecule 5-aminouracil, its equilibrium geometry and harmonic wavenumbers were calculated for the first time by the B3LYP DFT method. The vibrational wavenumbers were compared with IR and Raman experimental data. Also good reproduction of the experimental wavenumbers is obtained and the % error is very small. All the tautomeric forms of 5-aminouracil were determined and optimized. The dimer forms were also simulated. The energy, atomic charges and dipole moments were discussed and several general conclusions were underlined.     

Effect of Alkyl Chain Length of N-Alkyl-N′-(2-benzylphenyl)ureas on Gelation

Urea derivatives that were substituted with a 2-benzylphenyl group and an alkyl group functioned as low molecular weight gelators for various organic solvents and ionic liquids. Urea derivatives with long alkyl chains were effective for the gelation of polar solvents. However, they were not suitable for the gelation of non-polar solvents, whereas urea derivatives with short alkyl chains were effective. Ionic liquids were similar to polar solvents in that urea derivatives with long alkyl chains were the most effective gelators. The physical properties of the formed supramolecular gels were analyzed by dynamic viscoelasticity measurements using a rheometer.     

国标测定土壤中铅测定方法改进的探讨

为改进测定土壤中铅的石墨炉原子吸收法,通过湿法消解,应用基体改进剂磷酸二氢铵,提高方法的准确度和精密度.结果表明,方法的线性范围为0.0 ～ 50.0 μg/L,检出限为0.21mg/kg,回收率为82.6％～94.4％,该方法具有干扰因素少,灵敏度高、准确的特点,可推广应用.     

Polyimide-Silica Hybrids: Spectroscopy,Morphology and Mechanical Properties

Polyimide/silica hybrids were prepared by a sol-gel process and were evaluated in terms of curing behaviour, morphology and mechanical properties. The spectroscopic examination showed that the presence of the inorganic phase accelerates the imidization of the polyamic acid. Two types of morphology for the silica phase were obtained by tailoring the composition of the precursor solution mixture. The mechanical properties were found to be strongly dependent on the system morphology. The largest increase in rigidity and strength properties were achieved when the two phases were co-continuous.     

PET导电纤维的制取及研究

以过氧化二苯甲酰为引发剂,使丙烯睛在涤沦(PET)纤维上接枝共聚。接枝纤维在含铜化合物,含硫还原剂溶液中反应,制备PET导电纤维。讨论了影响接枝共聚的各种因素,选择出最佳聚合条件。对该纤维的导电成份和结构以及性能进行了研究。     

Preparation of Titania/PDMS Hybrid Films and the Conversion to Porous Materials

Transparent films of titania/poly(dimethylsiloxane) (PDMS) hybrids were prepared by the solvent evaporation from the precursor solution prepared by the co-hydrolysis and co-condensation of titanium tetraisopropoxide and a methoxy-functionalized PDMS. The hybrid films were flexible and had high homogeneity of the composition. The organic groups of PDMS were decomposed at 400°C in air to form porous films. Though the heated films were rather brittle compared to the as-synthesized films, they were still transparent and homogeneous. The BET surface areas of the films after the heat treatment at 400°C were over 300 m²/g, while the as-synthesized hybrid films were non porous. According to the BDDT classification, the nitrogen adsorption/desorption isotherms of the calcined films were Type I, showing that the films were microporous. The titania domains were still amorphous after the heat treatment at 400°C and transformed to anatase after the heat treatment at 1,000°C.