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Ultra-Rapid Crystallization of L-alanine Using Monomode Microwaves Indium Tin Oxide and Metal-Assisted and Microwave-Accelerated Evaporative Crystallization

机译:使用单模微波氧化铟锡和金属辅助微波加速蒸发结晶法对L-丙氨酸进行超快速结晶

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摘要

The use of indium tin oxide (ITO) and focused monomode microwave heating for the ultra-rapid crystallization of L-alanine (a model amino acid) is reported. Commercially available ITO dots (< 5 mm) attached to blank poly(methyl)methacrylate (PMMA, 5 cm in diameter with 21-well silicon isolators: referred to as the iCrystal plates) were found to withstand prolonged microwave heating during crystallization experiments. Crystallization of L-alanine was performed at room temperature (a control experiment), with the use of two microwave sources: a 2.45 GHz conventional microwave (900 W, power level 1, a control experiment) and 8 GHz (20 W) solid state, monomode microwave source with an applicator tip that focuses the microwave field to a 5-mm cavity. Initial appearance of L-alanine crystals and on iCrystal plates with ITO dots took 47 ± 2.9 min, 12 ± 7.6 min and 1.5 ± 0.5 min at room temperature, using a conventional microwave and focused monomode microwave heating, respectively. Complete evaporation of the solvent using the focused microwaves was achieved in 3.2 ± 0.5 min, which is ~52-fold and ~172-fold faster than that observed at room temperature and using conventional microwave heating, respectively. The size and number of L-alanine crystals was dependent on the type of the 21-well iCrystal plates and the microwave heating method: 33 crystals of 585 ± 137 μm in size at room temperature > 37 crystals of 542 ± 100 μm in size with conventional microwave heating > 331 crystals of 311 ± 190 μm in size with focused monomode microwave. FTIR, optical microscopy and powder X-ray diffraction analysis showed that the chemical composition and crystallinity of the L-alanine crystals did not change when exposed to microwave heating and ITO surfaces. In addition, theoretical simulations for the binding of L-alanine molecules to ITO and other metals showed the predicted nature of hydrogen bonds formed between L-alanine and these surfaces.
机译:据报道,铟锡氧化物(ITO)和聚焦单模微波加热用于L-丙氨酸(模型氨基酸)的超快速结晶。已发现连接到空白聚甲基丙烯酸甲酯(PMMA,直径为5厘米,具有21孔硅隔离器:称为iCrystal板)的市售ITO点(<5毫米)可承受结晶实验过程中长时间的微波加热。 L-丙氨酸的结晶在室温下进行(对照实验),使用两种微波源:2.45 GHz常规微波(900 W,功率水平1,对照实验)和8 GHz(20 W)固态的单模微波源,其喷头将微波场聚焦到5毫米腔中。在室温下,分别使用常规微波和聚焦单模微波加热,L-丙氨酸晶体和在带有ITO点的iCrystal板上的初始出现分别花费47±2.9分钟,12±7.6分钟和1.5±0.5分钟。使用聚焦微波在3.2±0.5分钟内实现了溶剂的完全蒸发,分别比在室温和常规微波加热下快约52倍和约172倍。 L-丙氨酸晶体的大小和数量取决于21孔iCrystal板的类型和微波加热方法:33个晶体在室温下的尺寸为585±137μm> 37个晶体,在尺寸上为542±100μm使用聚焦单模微波,常规微波加热> 331个311±190μm大小的晶体。 FTIR,光学显微镜和粉末X射线衍射分析表明,当暴露于微波加热和ITO表面时,L-丙氨酸晶体的化学组成和结晶度没有改变。此外,有关L-丙氨酸分子与ITO和其他金属结合的理论模拟表明,L-丙氨酸与这些表面之间形成的氢键具有预测的性质。

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