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71.
Summary New separation procedures for alkaloids of similar polarity and structure or of very different polarity and structure, based upon two-dimensional thin-layer chromatography on unmodified silica gel under mild conditions are described. Separation factors and separation mechanisms based on the structure of the bases and mobile phase composition are discussed for some examples of very efficient procedures.Proportions in solvent mixtures are v/v except where otherwise indicated. 相似文献
72.
Surface diffusion in reversed-phase liquid chromatography (RPLC) using silica gels bonded with C1 and C18 alkyl ligands of different densities was studied from the viewpoints of two extrathermodynamic relationships, i.e., enthalpy-entropy compensation (EEC) and linear free energy relationship (LFER). First, according to the four methods proposed by Krug et al., the values of surface diffusion coefficient (Ds) were analyzed to confirm that an actual EEC resulting from substantial physico-chemical effects takes place for surface diffusion. Then, it was also demonstrated that a LFER is observed between surface diffusion and the retention equilibrium. The establishment of EEC and LFER suggests a mechanistic similarity of molecular migration by surface diffusion, irrespective of the alkyl chain length and the densities of C1 and C18 ligands. Finally, a thermodynamic model for the LFER based on the real EEC was used to estimate Ds values under various RPLC conditions. The Ds values can be estimated with a mean square deviation of about 25–30%. The agreement between the Ds values estimated and those experimentally measured suggests that the total mass flux by surface diffusion consists of the two contributions due to C1 and C18 ligands and that the contribution of each ligand is proportional to the ligand density. 相似文献
73.
Cimpeanu V Parvulescu VI Amorós P Beltrán D Thompson JM Hardacre C 《Chemistry (Weinheim an der Bergstrasse, Germany)》2004,10(18):4640-4646
Heterogeneous catalytic oxidation of a series of thioethers (2-thiomethylpyrimidine, 2-thiomethyl-4,6-dimethyl-pyrimidine, 2-thiobenzylpyrimidine, 2-thiobenzyl-4,6-dimethylpyrimidine, thioanisole, and n-heptyl methyl sulfide) was performed in ionic liquids by using MCM-41 and UVM-type mesoporous catalysts containing Ti, or Ti and Ge. A range of triflate, tetrafluoroborate, trifluoroacetate, lactate and bis(trifluoromethanesulfonyl)imide-based ionic liquids were used. The oxidations were carried out by using anhydrous hydrogen peroxide or the urea-hydrogen peroxide adduct and showed that ionic liquids are very effective solvents, achieving greater reactivity and selectivity than reactions performed in dioxane. The effects of halide and acid impurities on the reactions were also investigated. Recycling experiments on catalysts were carried out in order to evaluate Ti leaching and its effect on activity and selectivity. 相似文献
74.
Viorica Lopez-Avila Janet Benedicto Emi Baldin Werner F. Beckert 《Journal of separation science》1992,15(3):160-164
Nineteen halogenated and/or nitrated diphenyl ethers (currently listed in EPA Method 8111) have been separated on a DB-5/ DB-1701 column pair connected to an inlet splitter and separate electron capture detectors. Retention times are included for 10 additional compounds evaluated for their suitability as internal standards or surrogate compounds for incorporation into Method 8111. Method reproducibility and linearity are discussed, and results are presented for extracts of two real samples spiked with the 19 diphenyl ethers and analyzed using the dual-column dual-detector arrangement. 相似文献
75.
Mingdeng Wei Kiyomi Okabe Hironori Arakawa Yesutake Teraoka 《Reaction Kinetics and Catalysis Letters》2002,77(2):381-387
SiO2 was modified by hexagonal mesoporous silica to form a mixture with meso-/macroporous sizes and used as support of Co catalysts for Fischer-Tropsch synthesis in a slurry phase. A synergistic effect on the activity of Co catalyst was found. The catalytic properties are related to the state of surface Co and the character of support. 相似文献
76.
《Journal of separation science》2003,26(8):701-708
A micellar electrokinetic chromatographic and a fast reversed‐phase liquid chromatographic method have been developed for determination of the purity of phenoxymethylpenicillin. The optimized running buffer composition was 40 mM phosphate–borate–125 mM SDS–3.5% (v/v) methanol. The HPLC method employed a monolithic silica C18 column and a mobile phase composed of phosphate buffer, pH 3.5, and ACN, the flow‐rate being 3.5 mL/min. Both methods were successfully validated. Linearity, intermediate precision, limits of quantitation, accuracy, and a good correlation of the HPLC and MEKC results were demonstrated. Both methods proved to be fast and reliable and sufficiently sensitive. A combination of the two methods can be very useful in impurity profiling. 相似文献
77.
Y. Akiyama F. Mizukami H. Izutsu M. Sato K. Maeda Y. Kiyozumi K. Sakaguchi 《Journal of Sol-Gel Science and Technology》1998,13(1-3):421-425
A novel organic-inorganic composite was prepared by a sol-gel process using hydrolysis and condensation of tetraethoxysilane (TEOS) reacted with a saccharide. During the process, ethoxy groups of the TEOS were replaced with hydroxyl groups of the saccharide and, consequently, saccharide molecules were combined with silica through their hydroxyl groups. Samples obtained under different reaction conditions were used for optical resolution of a metal chelate compound. The resolution ability of the composites was affected by the amount of water added for hydrolysis and of the saccharide. In particular, the amount of water drastically influenced the optical resolution performance. Composites obtained at the lower H2O/TEOS ratio gave the metal chelate compound a higher optical rotation. Three types of composites with the same composition were prepared by kneading, impregnation and by the sol-gel method, and were compared. The sol-gel composite showed the best optical resolution ability. It was concluded that the optical resolution ability was closely related to dispersibility of saccharide in the silica matrix. 相似文献
78.
Drying dissipative structural patterns formed in the course of drying colloidal crystals of silica spheres (110 nm in diameter)
in water, methyl alcohol, ethyl alcohol, 1-propyl alcohol, diethyl ether, and in the mixtures of ethyl alcohol with the other
solvents above have been studied on a cover glass. The macroscopic broad rings were formed in the outside edges of the dried
film for all the solvents examined. Furthermore, much distinct broad rings appeared in the inner area when the solvents were
ethyl alcohol, methyl alcohol, and their mixtures. Profiles of the thickness of the dried films were sensitive to the organic
solvents and explained well with changes in the surface tensions, boiling points, and viscosities of the solvents. The macroscopic
and microscopic spoke-like crack patterns formed. The drying area (or the drying time) increased (or decreased) as the surface
tension of the solvent decreased. However, the absolute values of these drying parameters are determined also by the boiling
points of the solvents. Importance of the fundamental properties of the solvents is supported in addition to the characteristics
of colloidal particles in the drying dissipative pattern formation. 相似文献
79.
高效液相色谱氮杂冠醚键合固定相的合成及性能研究 总被引:2,自引:0,他引:2
我们曾用γ-氯丙基键合硅胶(CPS),在氢化钠(NaH)作用下合成了3-(氮杂-18-冠-6)丙基键合固定相(BCP)[1].该固定相对碱基、核苷酸、硝基苯酚等有较好的分离选择性,但由于NaH对硅胶基质腐蚀作用较大,导致BCP柱效及渗透性较低.本文采... 相似文献
80.
Hartmut Hibst 《Angewandte Chemie (International ed. in English)》1982,21(4):270-282
Owing to their particular crystallographic properties, ferrimagnetic hexagonal ferrites exhibit a far greater coercive force than the conventional magnetic pigments. They therefore appear to be suitable for use in magnetic information storage procedures, some of which are novel and are at the development stage. Thus, magnetic tapes of high coercive force containing barium ferrite could be used as master tapes for copying magnetic information or for producing forgery-proof magnetic cards, if magnetic heads having high-order write fields were successfully developed. Moreover, platelet-like ferrite pigments in which the preferred direction of magnetic orientation is perpendicular to the plane of the platelet are of great interest for perpendicular magnetic recording. In this progress report, the crystal structures, magnetic characteristics of hexagonal ferrites, and chemical processes for their production are discussed. In particular, reactions in salt melts or under hydrothermal conditions produce finely divided pigments whose particles have a pronounced hexagonal, plate-like habit, a narrow particle size distribution, and advantageous magnetic properties. The magnetic properties of the pigments crystallized from salt melts may be adjusted by cation exchange. 相似文献