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151.
Capillary electrophoresis (CE) is becoming an established method for the determination of chiral trace impurities. This paper provides an overview of the state of the art of CE for such determinations. Detection limits of 0.1% impurity is widely accepted as a minimum requirement for chiral trace impurity determinations. This can be relatively easily achieved with CE. However, determination of lower concentrations requires careful optimization of the separation system. Four factors that are of particular significance for trace enantiomeric determinations: resolution, limit of detection, linear range and type of detection, are discussed. Further, the advantages and disadvantages of derivatization in this context are treated as well as the separation approach, ie., direct chiral separation or separation after the formation of diastereomers. It is concluded that the limit of impurity detection can be about 0.05% when UV detection is employed. Using laser-induced fluorescence detection, a quantitative determination at the 0.005% level is often possible. 相似文献
152.
聚合物假冠醚研究(Ⅰ)单体乙二醇二苯醚的合成与表征 总被引:1,自引:0,他引:1
本文以乙二醇为底物,通过中间体乙二醇二苯磺酸酯,合成出了乙二醇二苯醚。对两合成产物进行了红外光谱、薄层色谱。溶解性能及结晶分析,实验结果表明,在乙二醇二苯磺酸酯的合成中,因为使用苯磺酰氯代替了传统的对甲苯磺酰氯磺酰化试剂,并用氯仿做稀释剂以控制催化剂吡啶的恰当使用量,使合成不但经济而且获得82.5%,的较高收率,在乙二醇二苯醚的合成中,采用回流,蒸馏交替使用的实验方法,同时用馏出物沸点数值监控和及时排除体系的水份,使产率达到78.0%。 相似文献
153.
Hong-Ping Lin Yah-Ru Cheng Chung-Rong Lin Feng-Yin Li Chang-Lin Chen She-Tin Wong Soofin Cheng Shang-Bin Liu Ben-Zu Wan Chung-Yuan Mou Chin-Yuan Tang Ching-Yen Lin 《中国化学会会志》1999,46(3):495-507
We report a “delayed neutralization” process for the preparation of highly-ordered aluminosilicate MCM-41 molecular sieves with high thermal and hydrothermal stability, and sharp pore size distribution. However, the structural order and pore size are dependent on the carbon chain length. In the mixture surfactant systems, the pore size of the MCM-41 materials could be fine-tuned. The pore size can be extended from 2.5 to 4.5 nm by adding a suitable amount of hydrocarbons. The tubular morphology of the MCM-41 material of 0.3 to 10 micrometers diameter, where the wall consists of coaxial cylindrical pores of nanometers MCM-41, can be obtained by careful control of the surfactant-water content and the rate of condensation of silica. An optimum condition for automatic synthesis of the hierarchical TWT structure has been accomplished. The addition of 1-alkanols as cosurfactant would not only improve the order of the MCM-41 hexagonal structure but also promote the formation of micrometer-sized hierarchical materials, for example: tubules-within-tubule and uniform-sized hollow spheres of diameter 5.0 ± 1.0 μm. However, the inside of the micron spheres has intricate structures possessing various topological genus ranks. The MCM-41 is a good supporter for Molybdenum oxide catalysts. The rate of deactivation in the catalytic reaction of ethyl-benzene dehydrogenation to styrene increases in the order: MT < MP < SiO2. The physically mixed samples have higher catalytic activity than impregnated ones. 相似文献
154.
随着有机磷化合物(OPs)的广泛应用,其在越来越多的环境介质中被检测出来。大多数OPs具有毒性,但人们缺乏快速且有效的预测手段来对毒性进行评估。本文将结合E-Dragon软件计算的分子描述符,采用不同的QSAR模型对36个OPs的毒性进行预测。文中采用后退法作为描述符筛选方法,以均方根误差(RMSE)作为评价标准,共找到14个对线性核函数支持向量机(SVM)模型贡献较大的描述符;在最终得到的SVM模型交叉验证结果中,计算值与实际值的相关系数为0. 913,均方根误差为0. 388;外部测试验证结果中,平均相对误差为9. 10%。此外,采用多元线性回归(MLR)、人工神经网络(ANN)以及偏最小二乘回归(PLS)模型对OPs的毒性进行预测,交叉验证结果显示,三个模型的计算值与实际值的相关系数分别为0. 878、0. 686与0. 620,没有SVM模型的预测能力好。因此采用线性核函数的SVM模型对OPs进行毒性预测是一个行之有效的方法。 相似文献
155.
N doped TiO2 with anatase and rutile mixed crystal were prepared by using tetrabutyl titanate as the precursor via a modified hydrothermal process and calcination at 320 °C. The microstructure and morphology of samples were characterized by XRD, UV-vis-DRS, FTIR and XPS. The results showed that N-TiO2 particles were crystallized to anatase and rutile mixed crystal structure; they were presented narrow particle size distribution, and the average particle size was ca. 13.5 nm calculated from XRD results. It was found that the N-doped TiO2 particles showed strong visible-light absorption and high photocatalytic activity for the mineralization of Rhodamine B under irradiation by visible light (400-500 nm). The high visible-light photocatalytic activity of the obtained N-doped TiO2 might result from the synergetic effect of nitrogen doping and the mixed lattice structure of N-TiO2. Possible mechanism of N-TiO2 mixed crystal formed under hydrothermal conditions was discussed. 相似文献
156.
Wan Yong Feng Moshe Goldenberg Chava Lifshitz 《Journal of the American Society for Mass Spectrometry》1994,5(8):695-703
Thermal reactions of proton-bound dimers, (CH3CN)2H +, (CH3OCH3)2H +, and (CH3COCH3)2H+, were studied using a selected ion flow tube. Reactions observed include association, switching, and proton transfer. The association channel was observed only for base molecules that had hydrogen bonding protons such as NH3, CH3NH2, (CH3)2NH, and CH3OH. An association-insertion mechaniSoc was proposed in which the central proton of the symmetrically bound dimers is replaced by a protonated base, for example, NH 4 + . These reactions are relatively slow, which demonstrates a central barrier along the potential energy surface. Ether-containing dimers do not demonstrate this insertion reaction, except for diethers, for example, CH3OCH2CH2OCH3, which can form stable bicyclic structures. Dimers such as (HCOOH)2H+, which possess hydrogen bonding protons in the periphery, undergo switching reactions with ammonia and no insertion. 相似文献
157.
158.
159.
The effect of glottal angle on intraglottal pressure 总被引:1,自引:0,他引:1
Li S Scherer RC Wan M Wang S Wu H 《The Journal of the Acoustical Society of America》2006,119(1):539-548
Intraglottal pressure distributions depend upon glottal shape, size, and diameter. This study reports the effects of varying glottal angle on intraglottal and transglottal pressures using a three-dimensional Plexiglas model with a glottis having nine symmetric glottal angles and a constant minimal glottal diameter of 0.06 cm. The empirical data were supported by computational results using FLUENT. The results suggested that (1) the greater the convergent glottal angle, the greater outward driving forces (higher intraglottal pressures) on the vocal folds; (2) flow resistance was greatest for the uniform glottis, and least for the 10 degrees divergent glottis; (3) the greatest negative pressure in the glottis and therefore the greatest pressure recovery for diverging glottal shapes occurred for an angle of 10 degrees; (4) the smaller the convergent angle, the greater the flow resistance; (5) FLUENT was highly accurate in predicting the empirical pressures of this model; (6) flow separation locations (given by FLUENT) for the divergent glottis moved upstream for larger flows and larger glottal angles. The results suggest that phonatory efficiency related to aerodynamics may be enhanced with vocal fold oscillations that include large convergent angles during glottal opening and small (5 degrees - 10 degrees) divergent angles during glottal closing. 相似文献
160.
A cathode material of an electrically conducting carbon–LiFePO4 nanocomposite is synthesized by wet ball milling and spray drying of precursor powders prior to a solid-state reaction. The
structural characterization shows that the composite is composed of LiFePO4 crystals and 4.8 wt.% amorphous carbon. Galvanostatic charge/discharge measurements indicate that the composite exhibits
a superior high energy and high cycling stability. This composite delivers a discharge capacity of 159.1 mAh g−1 at 0.1 C, 150.8 mAh g−1 at 1 C, and 140.1 mAh g−1 at 2 C rate. The capacity retention of 99% is achieved after 200 cycles at 2 C. The 18,650 cylindrical batteries are assembled
using the composite as cathode materials and demonstrate the capacity of 1,400 mAh and the capacity retention of 97% after
100 cycles at 1 C. These results reveal that the as-prepared LiFePO4–carbon composite is one of the promising cathode materials for high-performance, advanced lithium-ion batteries directed
to the hybrid electric vehicle and pure electric vehicle markets. 相似文献