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1.
Surface modification of soft-glass capillaries for gas chromatography by treatment with water vapour
“Leaching” or “etching” by strong mineral acids seems to be a necessary pretreatment step for the most commonly used deactivation procedures of glass capillaries by reaction with either polyethylene glycol or silylation reagents. The acidic sites which are formed on the surface during this acid treatment cannot be completely removed by the subsequent deactivation process. This drawback can be overcome by performing the leaching with water vapour, resulting in an accumulation of cations at the surface and a decrease in the number of silanol groups. Capillaries of this type show excellent properties for the chromatography of strongly basic compounds. After the wash-out of the alkaline surface layer, the acidity of the support is suited for the chromatography of strongly basic as well as strongly acidic compounds. Due to a lack of reactive acidic sites, special deactivation procedures have to be applied to capillaries produced in this way. 相似文献
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Anusuya Choudhury Michael E. Pierce Dieu Nguyen Louis Storace Pat N. Confalone 《Tetrahedron letters》2005,46(47):8099-8102
D-D4FC (1) is an anti-HIV agent currently under phase II clinical trial (Pharmaset Inc). Its molecular architecture is suitable for a Ferrier rearrangement kind of operation on a furanoid glycal to fix the position of the double bond and the relative stereochemistry. Despite the fact that classical Ferrier rearrangement does not work on furanoid glycals, a palladium mediated modified protocol has been developed for the glycosidation of an aromatization prone xylo-furanoid glycal (5) for the synthesis of D-D4FC. 相似文献
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In view of existing contradictory assignments of the symmetrical stretching vibrations associated with the formal C-C and C-F bonds of trans/cis oxalyl fluoride, an additional theoretical analysis of the corresponding calculated wavenumbers was preformed on trans-C2O2F2 and cis-C2O2F2 based on previously calculated ab initio scaled force fields at the HF/6-31G computational level and new force fields calculated at the MP2/aug-cc-pVTZ level. This novel analysis included computational data from the isotopic shifts brought about by incorporating 13C and 14C atoms into the structure. A detailed examination of the calculated wavenumbers made it possible to validate the assignments of the ν2 and ν3 wavenumbers in the trans-C2O2F2 and cis-C2O2F2 molecules as the formal C-C bond stretching and the formal C-F bond symmetrical stretching vibrations, respectively. 相似文献
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Automated flow-based anion-exchange method for high-throughput isolation and real-time monitoring of RuBisCO in plant extracts 总被引:1,自引:0,他引:1
In this work, a miniaturized, completely enclosed multisyringe-flow system is proposed for high-throughput purification of RuBisCO from Triticum aestivum extracts. The automated method capitalizes on the uptake of the target protein at 4 °C onto Q-Sepharose Fast Flow strong anion-exchanger packed in a cylindrical microcolumn (105 × 4 mm) followed by a stepwise ionic-strength gradient elution (0-0.8 mol/L NaCl) to eliminate concomitant extract components and retrieve highly purified RuBisCO. The manifold is furnished downstream with a flow-through diode-array UV/vis spectrophotometer for real-time monitoring of the column effluent at the protein-specific wavelength of 280 nm to detect the elution of RuBisCO. Quantitation of RuBisCO and total soluble proteins in the eluate fractions were undertaken using polyacrylamide gel electrophoresis (PAGE) and the spectrophotometric Bradford assay, respectively. A comprehensive investigation of the effect of distinct concentration gradients on the isolation of RuBisCO and experimental conditions (namely, type of resin, column dimensions and mobile-phase flow rate) upon column capacity and analyte breakthrough was effected. The assembled set-up was aimed to critically ascertain the efficiency of preliminary batchwise pre-treatments of crude plant extracts (viz., polyethylenglycol (PEG) precipitation, ammonium sulphate precipitation and sucrose gradient centrifugation) in terms of RuBisCO purification and absolute recovery prior to automated anion-exchange column separation. Under the optimum physical and chemical conditions, the flow-through column system is able to admit crude plant extracts and gives rise to RuBisCO purification yields better than 75%, which might be increased up to 96 ± 9% with a prior PEG fractionation followed by sucrose gradient step. 相似文献
5.
Yurii N. Panchenko Charles W. Bock Joseph D. Larkin Alexander V. Abramenkov 《Structural chemistry》2008,19(5):793-799
In connection with the appearance of new experimental vibrational data on the high-energy rotational isomer of 2,3-dimethylbuta-1,3-diene
(I) in a low-temperature matrix and in neat crystals, the ab initio-based vibrational analysis of this molecule has been re-evaluated.
Calculated wavenumbers derived from a scaled quantum-mechanical force field analysis at the MP2(FC)/aug-cc-pVDZ//MP2(FC)/aug-cc-pVDZ
computational level are compared with experimental data. Several reassignments of the fundamental wavenumbers for I have been suggested in the course of the current analysis, and the existence of a high-energy non-planar s-gauche conformer of 2,3-dimethylbuta-1,3-diene has been confirmed. 相似文献
6.
Yu-jie Zhang Hong-guo Zhang Hong-wei Zhang Jing-lan Chen Guang-heng Wu 《Journal of magnetism and magnetic materials》2010,322(15):2251-809
A series of rare-earth doped BiFeO3 samples, Bi1−xRxFeO3 (x=0-1, R=La, Nd, Sm, Eu and Tb), were prepared in this work. X-ray diffraction analysis showed that the structure of rare-earth doped BiFeO3 was transformed from rhombohedral lattice to orthorhombic one by increasing x. The lattice constants and unit-cell volume decreased with the increasing of the doping content, while both the Néel temperature and magnetization were enhanced. A magnetic phase transition was observed at about 35 K for BiFeO3. The variation of the magnetization with temperature depended on applied field strength and magnetizing history, which was explained according to the antiferromagnetic exchange interaction between Fe and R sites in Bi1−xRxFeO3(x>0). The magnetocrystalline anisotropy contributed by Fe sublattice gave rise to a large coercivity in BixNd1−xFeO3 with an orthorhombic structure. 相似文献
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Pesticide residue in vegetables has been considered as a serious food safety problem across the whole world. This study investigates a novel advanced oxidation process (AOP), namely the coupled free chlorine/ultrasound (FC/US) process for the removal of three typical pesticides from lettuce. The removal efficiencies of dimethoate (DMT), trichlorfon (TCF) and carbofuran (CBF) from lettuce reached 86.7%, 79.8% and 71.3%, respectively by the FC/US process. There existed a synergistic effect in the coupled FC/US process for pesticide removal and the synergistic factors reached 22.3%, 19.0% and 36.4% for DMT, TCF and CBF, respectively. Based on the analysis of mass balance of pesticides, the synergistic effect was probably attributed to the efficient oxidation of pesticides both in vegetables and in water by the generated free radicals and FC. The surface area and surface structure of vegetables strongly affected the removal of pesticides by FC/US. The removal efficiency of DMT increased from 80.9% to 88.1% as solution pH increased from 5.0 to 8.0, and then decreased to 84.1% when solution pH further increased to 9.0. When the ultrasonic frequency changed from 20 to 40 kHz, a remarkable improvement in pesticide removal by FC/US was observed. As the FC concentration increased from 0 to 15 mg L–l, the removal efficiencies of pesticides increased firstly, and then became stagnant when the FC concentration further increased to 25 mg L–l. The pesticide degradation pathways based on the identified intermediates were proposed. The total chlorophyll content was reduced by less than 5% after the FC/US process, indicating a negligible damage to the quality of vegetables. It suggests that the FC/US process is a promising AOP for pesticides removal from vegetables. 相似文献
10.
倒装芯片塑料球栅阵列(FC-PBGA)封装形式独特而被广泛应用, 分析研究其在实际应用过程中, 在高温、电、水汽等多种综合环境应力条件作用下的失效机理对提高其应用可靠性有重要意义. 本文对0.13 μm 6层铜布线工艺的FC-PBGA FPGA器件, 通过暴露器件在以高温回流焊过程中的热-机械应力为主的综合外应力作用下的失效模式, 分析与失效模式相对应的失效机理. 研究结果表明, FC-PBGA器件组装时的内外温差及高温回流焊安装过程中所产生的热-机械应力是导致失效的根本原因, 在该应力作用下, 芯片上的焊球会发生再熔融、桥接相邻焊球致器件短路失效; 芯片与基板之间的填充料会发生裂缝分层、倒装芯片焊球开裂/脱落致器件开路失效; 芯片内部的铜/低k互连结构的完整性受损伤而影响FC-PBGA器件的使用寿命. 相似文献