Preparation of polysiloxane stationary phases for capillary column chromatography: A New methoxyphenyl phase

Contemporary methods for the synthesis of alkyl- and arylsubstituted polysiloxane stationary phases are reviewed. A new, moderately polar phase containing the 3-(4-methoxyphenyl)-propyl group is reported.     

Cyclocarbonylation of unsaturated tosylates as a method of cyclanone synthesis

A study has been made to determine the scope of the cyclocarbonylation reaction of olefinic tosylates with Na₂Fe(CO)₄.     

On the problem of periodicity and hidden solitons for the KdV model

In continuum limit, the Fermi-Pasta-Ulam lattice is modeled by a Korteweg-de Vries (KdV) equation. It is shown that the long-time behavior of a KdV soliton train emerging from a harmonic excitation has a regular periodicity of right- and left-going trajectories. In a soliton train not all the solitons are visible, the solitons with smaller amplitude are hidden and their influence is seen through the changes of phase shifts of larger solitons. In the case of an external harmonic force several resonance schemes are revealed where both visible and hidden solitons have important roles. The weak, moderate, strong, and dominating fields are distinguished and the corresponding solution types presented.     

Thermal marks as a signal processing aid for a portable capillary electropherograph

The interpretation of raw signals in capillary CE can be challenging if there are unknown peaks, or the signal is corrupt due to baseline fluctuations, EOF velocity drift, etc. Signal processing could be required before results can be interpreted. A suite of signal processing algorithms has been developed for CE data analysis, specifically for use in field experiments for the detection of nerve agents using portable CE instruments. Everything from baseline correction and electropherogram alignment to peak matching and identification is included in these programs. Baseline correction is achieved by interpolating a new baseline according to points found using all local extremes, by applying an appropriate outliers test. Irreproducible migration times are corrected by compensating for EOF drift, measured with the aid of thermal marks. Thermal marks are small disturbances in the capillary created by punctual heating that move with the velocity of EOF. Peaks in the sample electropherogram are identified using a fuzzy matching algorithm, by comparing peaks from the sample electropherogram to peaks from a reference electropherogram.     

Waves in microstructured solids and the Boussinesq paradigm

The emergence of soliton trains and interaction of solitons are analyzed by using a Boussinesq-type equation which describes the propagation of bi-directional deformation waves in microstructured solids. The governing equation in the one-dimensional setting is based on the Mindlin model. This model includes scale parameters which show explicitly the influence of the microstructure in wave motion. As a result the governing equation has a hierarchical structure. The analysis is based on numerical simulation using the pseudospectral method. It is shown how the number of solitons in emerging trains depends on the initial excitation. The head-on collision of emerged solitons is not fully elastic due to radiation but the solitons preserve their identity after collision and the speed of solitons is retained while the radiation keeps a certain mean value. That is why we have kept through this paper the notion of solitons.     

Monitoring of the electroosmotic flow of ionic liquid solutions in non-aqueous media using thermal marks

The possibility of applying a new method employing thermal marks to measuring the rate of the electroosmotic flow (EOF) in non-aqueous capillary electrophoresis (NACE) was investigated. The thermal marks were monitored by using a contactless conductivity detection. During one experiment and in between the series of experiments the reproducibility of the method was excellent. The EOF rate was measured 4-7 times during one experiment, the precision of measurement being around 0.5%. In this study, the influence of 1-butyl-3-methyl-imidazolium salts in organic solvents on the rate of the EOF was investigated. Various organic solvents were mixed with an ionic liquid of various concentrations and the EOF rate was measured using thermal marks. The accuracy of the method was compared with that of the neutral marker one. Five benzoic acid derivatives were separated while the EOF was monitored. The relative standard deviations of the corrected effective mobilities of the above analytes were in the range of 1.0-6.1%.     

Ammine magnesium borohydride complex as a new material for hydrogen storage: structure and properties of Mg(BH4)2.2NH3

The ammonia complex of magnesium borohydride Mg(BH4)2.2NH3 (I), which contains 16.0 wt % hydrogen, is a potentially promising material for hydrogen storage. This complex was synthesized by thermal decomposition of a hexaaammine complex Mg(BH4)2.6NH3 (II), which crystallizes in the cubic space group Fm3 m with unit cell parameter a=10.82(1) A and is isostructural to Mg(NH3) 6Cl2. We solved the structure of I that crystallizes in the orthorhombic space group Pcab with unit cell parameters a=17.4872(4) A, b=9.4132(2) A, c=8.7304(2) A, and Z=8. This structure is built from individual pseudotetrahedral molecules Mg(BH4)2.2NH3 containing one bidentate BH4 group and one tridentate BH4 group that pack into a layered crystal structure mediated by N-H...H-B dihydrogen bonds. Complex I decomposes endothermically starting at 150 degrees C, with a maximum hydrogen release rate at 205 degrees C, which makes it competitive with ammonia borane BH 3NH3 as a hydrogen storage material.