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121.
Jun D Stodulka P Kuca K Koleckar V Dolezal B Simon P Veverka M 《Journal of chromatographic science》2008,46(4):316-319
In this study, several thin-layer chromatography (TLC) methods are described for the identification of quaternary and non-quaternary compounds (parent compounds, intermediates, by-products, and products) arisen within the synthesis of the acetylcholinesterase reactivator HI-6, at present the most promising antidote in the case of nerve agent poisonings. Using the TLC technique, particular E and Z isomers of this compound on the oxime group are separated. These TLC methods could be of high interest as quick purity control for those who are interested in development of new acetylcholinesterase reactivators and the synthesis of HI-6 in laboratories or in large-scale production. 相似文献
122.
Simul 6 is a 1D dynamic simulator of electromigration based on the mathematical model of electromigration in free solutions. The model consists of continuity equations for the movement of electrolytes in a separation channel, acid–base equilibria of weak electrolytes, and the electroneutrality condition. It accounts for any number of multivalent electrolytes or ampholytes and provides a complete picture about dynamics of electromigration and diffusion in the separation channel. The equations are solved numerically using software means which allow for parallelization and multithreaded computation. Simul 6 has a user-friendly graphical interface. It is typically used for inspection of system peaks (zones) in electrophoresis, stacking and preconcentrating analytes, optimization of separation conditions, method development in either capillary zone electrophoresis, isotachophoresis, and isoelectric focusing. Simul 6 is the successor of Simul 5, and has been launched as a free software available for download at https://simul6.app/ . 相似文献
123.
Elisseos Verveniotis Emil Šípek Jiří Stuchlík Jan Kočka Bohuslav Rezek 《Journal of Non》2012,358(17):2118-2121
We describe two successful routes for generating ordered arrays of Si nanocrystals by using atomic force microscopy (AFM) and amorphous silicon thin films (200–400 nm) on Ti/Ni coated glass substrates. First, we show that field-enhanced metal-induced solid phase crystallization at room temperature can be miniaturized to achieve highly spatially localized (below 100 nm) current-induced crystallization of the amorphous silicon films using a sharp tip in AFM. In the second route, resistive nano-pits are formed at controlled positions in the amorphous silicon thin films by adjusting (lowering and/or stabilizing) the exposure currents in the AFM process. Such templated substrates are further used to induce localized growth of Si nanocrystals in plasma-enhanced chemical vapor deposition process. In both cases the crystalline phase is identified in situ as features of enhanced current in current-sensing AFM maps. 相似文献
124.
We introduce a computer implementation of the mathematical model of capillary zone electrophoresis described in the previous paper in this issue (Hru?ka et al., Electrophoresis 2012, 33), the program PeakMaster 5.3. The computer model calculates eigenmobilities, which are the eigenvalues of the Jacobian matrix of the electromigration system, and which are responsible for the presence of system eigenzones (system zones, system peaks). The model also calculates parameters of the background electrolyte: pH, conductivity, buffer capacity, ionic strength, etc., and parameters of the separated analytes: effective mobility, transfer ratio, molar conductivity detection response, and relative velocity slope. In addition to what was possible in the previous versions of PeakMaster, Version 5.3 can predict the shapes of the system peaks even for a complex injected sample profile, such as a rectangular plug. PeakMaster 5.3 can replace numerical simulation in many practically important configurations and the results are obtained in a very short time (within seconds). We demonstrate that the results obtained in real experiments agree well with those calculated by PeakMaster 5.3. 相似文献
125.
Simulation of the effects of complex- formation equilibria in electrophoresis: I. mathematical model
Simul 5 Complex is a one-dimensional dynamic simulation software designed for electrophoresis, and it is based on a numerical solution of the governing equations, which include electromigration, diffusion and acid-base equilibria. A new mathematical model has been derived and implemented that extends the simulation capabilities of the program by complexation equilibria. The simulation can be set up with any number of constituents (analytes), which are complexed by one complex-forming agent (ligand). The complexation stoichiometry is 1:1, which is typical for systems containing cyclodextrins as the ligand. Both the analytes and the ligand can have multiple dissociation states. Simul 5 Complex with the complexation mode runs under Windows and can be freely downloaded from our web page http://natur.cuni.cz/gas. The article has two separate parts. Here, the mathematical model is derived and tested by simulating the published results obtained by several methods used for the determination of complexation equilibrium constants: affinity capillary electrophoresis, vacancy affinity capillary electrophoresis, Hummel-Dreyer method, vacancy peak method, frontal analysis, and frontal analysis continuous capillary electrophoresis. In the second part of the paper, the agreement of the simulated and the experimental data is shown and discussed. 相似文献
126.
A novel procedure for the determination of stability constants in systems with neutral analytes and charged complexation agents by affinity capillary electrophoresis was established. This procedure involves all necessary corrections to achieve precise and reliable data. Temperature, ionic strength, and viscosity corrections were applied. Based on the conductivity measurements, the average temperature of the background electrolyte in the capillary was kept at the constant value of 25°C by decreasing the temperature of the cooling medium. The viscosity correction was performed using the viscosity ratio determined by an external viscosimeter. The electrophoretical measurements were performed, at first, at constant ionic strength. In this case, the increase of ionic strength caused by increasing complexation agent concentration was compensated by changing of the running buffer concentration. Subsequently the dependence of the analyte effective mobility on the complexation agent concentration was measured without the ionic strength compensation (at variable ionic strength). The new procedure for determination of the stability constants even from such data was established. These stability constants are in a very good agreement with those obtained at the constant ionic strength. The established procedure was applied for determination of the thermodynamic stability constants of (R, R)-(+)- and (S, S)-(-)-hydrobenzoin and R- and S-(3-bromo-2-methylpropan-1-ol) complexing with 6-monodeoxy-6-mono(3-hydroxy)propylamino-β-cyclodextrin hydrochloride. 相似文献
127.
Jana Svobodová Martin Beneš Pavel Dubský Gyula Vigh Bohuslav Gaš 《Electrophoresis》2012,33(19-20):3012-3020
This paper describes the results of the second‐level testing of the simulation program Simul 5 Complex. We compare the published experimental results with the simulated migration behavior of the enantiomers at different pH and chiral selector concentration values and use the same optimization object function, separation selectivity, as the original papers. Simul 5 Complex proved to be a suitable tool for the prediction of the effective mobilities, separation selectivities, and migration order reversals in these pH‐dependent and CD concentration dependent enantiomer separations. In addition, by performing simulations of four different separations systems (both real and model systems), Simul 5 Complex revealed the existence of unexpected and hitherto unexplained electromigration dispersion effects that were caused by the complexation process itself and could significantly impair the quality of the separations. 相似文献
128.
129.
Optimization of background electrolytes for capillary electrophoresis: II. Computer simulation and comparison with experiments 总被引:1,自引:0,他引:1
A mathematical and computational model described in the previous paper (Gas, B., Coufal, P., Jaros, M., Muzikár, J., Jelínek, L., J. Chromatogr. A 2001, 905, 269-279) is adapted, algorithmized, and a computer program PeakMaster having a status of freeware (http://natur.cuni.cz/ approximately gas) is introduced. The model enables optimization of background electrolyte (BGE) systems for capillary zone electrophoresis. The model allows putting to use uni- or di- or trivalent electrolytes and allows also for modeling highly acidic or alkaline BGEs. It takes into account the dependence of ionic mobilities and dissociation of weak electrolytes on the ionic strength. The model calculates the effective mobility of analytes and predicts parameters of the system that are experimentally available, such as the transfer ratio, which is a measure of the sensitivity in the indirect UV detection or the molar conductivity detection response, which expresses the sensitivity of the conductivity detection. Further, the model enables evaluation of a tendency of the analyte to undergo electromigration dispersion or peak broadening. The suitability of the model is verified by comparison of the predicted results with experiments, even under conditions that are far from ideal (under extreme pH and a high ionic strength). 相似文献
130.
The mobilities of the monocharged permanent tertraphenylphosphonium cation and tetraphenylborate anion are determined by capillary zone electrophoresis in different organic solvents as a function of the ionic strength, I, of the background electrolyte. The nonaqueous solvents are propylene carbonate (PC), N,N-dimethylformamide (DMF), N,N,-dimethylacetamide (DMA), acetonitrile (MeCN) and methanol (MeOH). The ionic strength is between 5 and 50 mmol/L. The mobility as a function of I is in good agreement with the theory of Debye, Hückel and Onsager (DHO), extended by the ion size parameter as introduced by Falkenhagen and Pitts. The values of the limiting DHO slopes of the mobility vs. I curves (the slopes express the influence of the solvent on the reduction of the mobility with increase of I) decrease in the order MeCN > MeOH > DMF > DMA > PC. Absolute mobilities (obtained by extrapolation to I = 0) of a particular ion differ by a factor of about 7 between the solvents. However, constancy within 10% is observed for their Walden products (the absolute mobility multiplied with the solvent's macroviscosity). The role of dielectric friction on the mobility of the present monocharged, large analyte ions is discussed according to the theory of Hubbard and Onsager. Based on the radii of the ions, the static permittivity of the solvent and its permittivity at infinite frequency, and the relaxation time of polarization, an equal contribution of dielectric and hydrodynamic friction is predicted in MeOH as solvent. Experimental data are in contrast to this prediction, indicating the overestimation of dielectric friction, and the dominance of hydrodynamic friction on the migration of the analyte ions in all solvents under consideration. 相似文献