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81.
《合成通讯》2013,43(11):2117-2126
Abstract Solvent‐free reactions of C60 and C70 with diethyl bromomalonate in the presence of various inorganic bases were investigated under the high‐speed vibration milling (HSVM) conditions, and are shown to give methanofullerenes 1 and 2 in good to excellent yields based on consumed fullerenes. Several weak inorganic bases were found to be quite effective in promoting the solvent‐free mechanochemical Bingel reactions of C60 and C70 under the HSVM conditions. Among the studied bases, sodium acetate gave the highest yield of monoadducts, while potassium carbonate afforded a considerable amount of bisadducts for both C60 and C70. 相似文献
82.
Supercritical fluid extraction (SFE) coupled with high‐speed counter‐current chromatography (HSCCC) was successfully used for the extraction and online isolation of the unstable compounds from Rosa damascene in a single extraction and separation operation in two stages. The solvent systems of SFE/HSCCC were optimized with the help of multiexponential function model. At the first stage, the upper phase of the solvent system of n‐butanol–tert‐butyl methyl ether–acetonitrile–0.1% aqueous TFA (1.7:1.0:0.8:4.0, v/v/v/v) was used as both the SFE entrainer and the HSCCC stationary phase, and the target compounds were eluted with the corresponding lower phase to separate the hydrophobic compounds. At the second stage, the upper phase of the solvent system of n‐hexane–ethyl acetate–methanol–water (3.2:1.0:2.8:2.6, v/v/v/v) was used as both the SFE entrainer and the HSCCC stationary phase, followed by elution with the corresponding lower phase to separate the moderate hydrophobic compounds. Six compounds including formononetin, delphinidin, cyaniding, 5,6,4′‐trihydroxy‐7,8‐dimethoxy flavone, 5,3′‐dihydroxy‐7,8‐dimethoxy flavone, and 5‐hydroxy‐6,7,8,3′,4′‐pentamethoxy flavone were successfully separated in one extraction–separation operation within 300 min. The targeted compounds were identified by MS and NMR spectroscopy. This research has opened up great prospects for industrial application of SFE/HSCCC to the extraction and separation of unstable compounds. 相似文献
83.
Chu Chu Shidi Zhang Shengqiang Tong Xingnuo Li Jizhong Yan 《Journal of separation science》2013,36(24):3958-3964
An efficient strategy for extracting and separating five lignans from Schisandra chinensis (Turcz.) Baill has been developed using supercritical fluid extraction (SFE) and high‐speed counter‐current chromatography (HSCCC) in the present study. First, the extraction was performed by a preparative SFE system under 15 MPa of pressure at 36°C for 4 h. Then, the SFE extract was successfully separated and purified by HSCCC with a two‐phase solvent system composed of n‐hexane/ethyl acetate/methanol/water (6:4:5:5, 6:4:6:4, 6:4:8:2, v/v) in a stepwise elution mode. The fractions were analyzed by HPLC, and the chemical structures of the products were identified by ESI‐MS and 1H NMR spectroscopy. As a result, a total of 12.5 mg of schisandrin at 98.0% purity, 7.1 mg of gomisin A at 98.1% purity, 1.8 mg of schisantherin B at 93.3% purity, 4.4 mg of deoxyschisandrin at 92.9% purity, and 6.8 mg of γ‐schisandrin at 89.1% purity were obtained from 300 mg crude extract in a one‐step purification. 相似文献
84.
Fast separations are very desirable in laboratories that analyze large numbers of samples per day or those needing short turn‐around times. Traditional HPLC methods using conventional stationary phases and standard column dimensions require significant amounts of organic solvents and generate large volumes of waste. With growing awareness about the environment, the development of green technologies has been receiving increasing attention. In this work, a very fast green analytical method based on LC‐UV using a short narrow bore column packed with fully porous sub‐2 μm particles has been developed for simultaneous determination of nine pharmaceuticals in wastewater and surface water. The chromatographic separation was optimized in order to achieve short analysis time and good resolution for all analytes in a single run. All analytes could be separated in 1 min with good resolution. Sample preparation was executed by solid phase extraction using Oasis HLB cartridges. The method developed was validated based on parameters such as linearity, precision, accuracy, detection, and quantification limits. The recovery ranged from 70.9 to 92.5% with SDs not higher than 5.4%, except for acetaminophen and sulphanilamide. LODs ranged from 0.6–2.5 μg/L, while the LOQs were in the range 2–8 μg/L. 相似文献
85.
Charlene S. Chua Simon P. A. Higgins Andreas Fouras 《Journal of synchrotron radiation》2010,17(5):624-630
A high‐repetition‐rate mechanical shutter with asynchronous control and sub‐millisecond operation has been developed and tested for specialist X‐ray systems in the field of medical diagnostics and radiation therapy. Capacitor‐coupled linear voice coil actuators are utilized to achieve opening and closing speeds as fast as 700 µs for an aperture height of 4 mm. The design allows for asynchronous control, permitting slave operation of the shutter, a feature that is distinctly suitable for a number of applications including particle image velocimetry, where high‐frame‐rate operation must be accurately synchronized and triggered by the image acquisition sequence of the detector or timing device. The design and construction of the shutter also makes it ideal, with simple and limited modifications, for applications requiring larger apertures, in particular wide beams as found in many synchrotron beamlines. 相似文献
86.
研究了以剩余寿命作为增补变量,排队空间有限的M/G/1排队模型,利用泛函分析中线性算子半群的积分半群理论讨论了该模型的瞬态解的存在唯一性问题。 相似文献
87.
With the introduction of wireless modems and smart phones, the passenger transport industry is witnessing a high demand to ensure not only the safety of the trains, but also to provide users with Internet access all the time inside the train. When the Mobile Terminal (MT) communicates directly with the Base Station (BS), it will experience a severe degradation in the Quality of Service due to the path loss and shadowing effects as the wireless signal is traveling through the train. In this paper, we study the performance in the case of relays placed on top of each train car. In the proposed approach, these relays communicate with the cellular BS on one hand, and with the MTs inside the train cars on the other hand, using the Long Term Evolution (LTE) cellular technology. A low complexity heuristic LTE radio resource management approach is proposed and compared to the Hungarian algorithm, both in the presence and absence of the relays. The presence of the relays is shown to lead to significant enhancements in the effective data rates of the MTs. In addition, the proposed resource management approach is shown to reach a performance close to the optimal Hungarian algorithm. 相似文献
88.
89.
The aim of the present study was to form a nitride layer on a titanium (Ti) substrate through a compact laser-nitriding system comprising a focused pulsed Nd:YAG laser and nitrogen gas blow. To obtain a high-quality layer, the effects of pulse frequency and gas flow rate on the surface characteristics were investigated by using plasma emission analysis as well as X-ray analyses. Optical emission spectra from the laser-induced plasma mainly consisted of ionic Ti lines, and their intensities when the pulse frequency was 15 Hz were much higher than those for 8 Hz. Similarly, the reflections from the δ-TiN phase in the X-ray diffraction (XRD) pattern were enhanced when using 15 Hz. On the other hand, the flow rate of nitrogen gas blow had a significant effect on the thickness of the thin oxide layer that formed above the nitride layer. Using a lower flow rate resulted in the formation of a thicker oxide layer. The higher pulse frequency and the faster flow rate were beneficial for obtaining a higher-quality layer because of the enhancement of nitridation and the suppression of oxidation, respectively. 相似文献
90.
通过电化学测试、 扫描电子显微镜观察和X射线衍射分析研究了电解液流速、 电流密度和锌沉积面容量三者关系及对锌镍单液流电池充放电性能和负极锌沉积形貌的影响. 结果表明, 锌沉积面容量是影响锌镍单液流电池充放电效率和负极锌沉积形貌的最主要因素, 电解液流速不宜过高或过低. 随着锌沉积面容量的增大, 电池的充放电效率和循环稳定性对电流密度的变化更为敏感, 适宜的电解液流速范围变窄. 锌沉积面容量在25 mA·h/cm2以上, 锌沉积皆呈海绵状. 在较低锌沉积面容量下, 电解液流速也较低时, 海绵锌沉积较为均匀致密. 而在高的锌沉积面容量下, 海绵状锌沉积的团簇和颗粒变大, 不均匀性加重, 仅在适中的电解液流速(7.1 L/min)下, 锌沉积部分致密规整, 电池具有较好的充放电性能. 相似文献