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81.
Improved quantification limits in chiral capillary electrochromatography by peak compression effects
The peak compression effect has been applied to improve quantification limits in chiral capillary electrochromatography (CEC). A stationary phase based on the chiral selector vancomycin (Chirobiotic V) was used for separations of the enantiomers of mianserin. By adding solvents with a low dielectric constant, e.g. 2-propanol or tetrahydrofuran, to the sample solution, peak compression could be induced. The plate numbers for the minor enantiomer increased from approximately 100,000 to 1.4-1.6 million plates/m, when the composition of the mobile phase was adjusted so that the analyte eluted within either one of two system zones originating from the sample solution. A 10-fold improvement in the quantification limit for the minor enantiomer was obtained compared to elution under non-focused conditions. 相似文献
82.
Korolev A Victorova E Ibragimov T Kanatyeva A Kurganov A 《Journal of separation science》2012,35(8):957-963
Monolithic capillary columns based on divinylbenzene were synthesized using different alcanols as porogens. Prepared columns were tested in separation of polystyrene standards according to their molar mass (MM) and were characterized by corresponding calibration graphs. It was demonstrated that a decrease of alcanol chain length from dodecanol to octanol resulted in a decrease of column permeability and in an improved column ability to separate polystyrene standards. In contrast, removing a good solvent from porogen mixture results in an increase of column permeability and in a decrease of column performance toward polystyrene standards. Optimized synthetic conditions included porogen composed of nonanol and toluene or mesytilene, and the column prepared with this porogen was capable of separating a mixture of 14 polystyrene standards with MM ranged from several millions to oligomers. 相似文献
83.
Kioumars Aghapoor Hossein Reza Darabi Kourosh Tabar-Heydar 《Phosphorus, sulfur, and silicon and the related elements》2013,188(5):1183-1187
On the benzyl system, bearing various functional groups, have been carried out the Willgerodt-Kindler reaction to obtain thiobenzmorpholide ( 1 ). The reactions, under solvent-free conditions, were performed in both classical (reflux, room temperature) and nonclassical (microwave) conditions to attempt our elucidation of the reactions pathways. Unlike benzylamine and benzyl mercaptan, benzyl halides give poor result due to the type of amine. The experimental results suggest that the proposed reaction pathway involves the oxidation coupling of benzylic substrates, followed by a thiolation step and an attack of the amine on the thiolated product to give ( 1 ). 相似文献
84.
Abbas Shockravi Hashem Shargi Hassan Valizadeh Majid M. Heravi 《Phosphorus, sulfur, and silicon and the related elements》2013,188(11):2555-2559
An efficient synthesis of 3-substituted coumarins under solventless system is described. 相似文献
85.
Majid M. Heravi Hossein A. Oskooie Ladan Sangsefidi Mitra Ghassemzadeh Koroush Tabar-Hydar 《Phosphorus, sulfur, and silicon and the related elements》2013,188(12):2843-2846
Oxidative deprotection of tetrahydropyranyl ethers (THP ethers) using chromium trioxide supported onto zeolite under microwave irradiation in solvent free condition is described. 相似文献
86.
Mahmood Tajbakhsh Majid M. Heravi Abolfazl Hosseini Ahmad Shahrezaiee 《Phosphorus, sulfur, and silicon and the related elements》2013,188(4):773-776
Hantzsch 1,4-dihydropyriines were rapidly and efficiently oxidized using bismuth nitrate supported onto silica gel under microwave irradiation. 相似文献
87.
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An electronic gas-flow controller system called Advanced Flow Control (AFC), which controls not only carrier gas pressure at the column inlet but also the total gas flow including the split flow, was designed and evaluated. BASIC programming of repetitive analyses of standard mixtures under varied split ratios and pressure programs allowed automated optimization of those conditions for the desired column loading and resolution between adjacent peaks. 相似文献
90.
叙述了CAHN-2000磁天平(美国)调试过程中如何解决液氮温区的测试,自制了磁天平与计算机的接口,编写了数据采集、处理和控制等高原 软件,节省了几万美元,部分指标超过原配套水平,三年来仪器在对国同外开放过程中,液氮温区的工作一直正常,实测了上千个样品,提供的数据已撰写数十篇文章在国内外刊物上发表。由此说明,要充分发挥进口仪器的使用效率,必须对仪器的工作原理、结构特点有透乇的了解,同时要有相当的自 相似文献