Publications by authors named "Jozef Sestak"

Efficient absorbance detection of a low-volume chromatography peak is a difficult task. In this work, an improved design of the fused silica capillary flow cell for absorbance detection in microcolumn liquid chromatography is described. The cell was fabricated from 0.

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Optical detection setup utilizing light emitting diodes (LEDs), 50 nL L-shaped silica capillary detection cell (L-cell), and low-cost CCD spectrometer is described in this work. Experimental configuration can be equipped with two different LEDs for absorbance measurement and other two LEDs for fluorescence excitation. This setup is capable of simultaneous multi-wavelength monitoring of absorbance and fluorescence when light produced by the individual LEDs and light emitted by the fluorescent analytes is resolved in the spectrum outputted by the CCD spectrometer.

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Miniaturised photometric detection cell based on the 150 μm I. D. L-shaped fused silica capillary (L-cell) and silica optical fibre is discussed in this paper.

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Head-column field-amplified sample stacking of cations from a low conductivity sample followed by enantiomeric separation using negatively charged chiral selectors was studied experimentally and with computer simulation. Aspects investigated include the direct electrokinetic injection of the analytes into the background electrolyte, the use of a selector free buffer plug, the contribution of complexation within the buffer plug and the application of an additional water plug between sample and buffer plug. Attention was paid for changes of ionic strength which is known to have a significant impact on complexation and thus effective mobility.

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Part I on head-column field-amplified sample stacking comprised a detailed study of the electrokinetic injection of a weak base across a short water plug into a phosphate buffer at low pH. The water plug is converted into a low conductive acidic zone and cationic analytes become stacked at the interface between this and a newly formed phosphoric acid zone. The fundamentals of electrokinetic processes occurring thereafter were studied experimentally and with computer simulation and are presented as part II.

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The fundamentals of electrokinetic injection of the weak base methadone across a short water plug into a phosphate buffer at low pH were studied experimentally and with computer simulation. The current during electrokinetic injection, the formation of the analyte zone, changes occurring within and around the water plug and mass transport of all compounds in the electric field were investigated. The impact of water plug length, plug injection velocity, and composition of sample, plug and background electrolyte are discussed.

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The synthesis and characterization of large-bore silica-based monolithic capillary columns (0.32mm×150mm) are presented. Columns were prepared by acidic hydrolysis of a mixture containing tetramethoxysilane (TMOS) and 1,2-bis(trimethoxysilyl)ethane (BTME) in different molar ratios in the presence of polyethylene glycol and urea.

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The electro-osmotic flow, a significant factor in capillary electrophoretic separations, is very sensitive to small changes in structure and surface roughness of the inner surface of fused silica capillary. Besides a number of negative effects, the electro-osmotic flow can also have a positive effect on the separation. An example could be fused silica capillaries with homogenous surface roughness along their entire separation length as produced by etching with supercritical water.

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The history of liquid chromatography started more than a century ago and miniaturization and automation are two leading trends in this field. Nanocolumn liquid chromatography (nano LC) and largely synonymous capillary liquid chromatography (capillary LC) are the most recent results of this process where miniaturization of column dimensions and sorbent particle size play crucial role. Very interesting results achieved in the research of extremely miniaturized LC columns at the end of the last century lacked distinctive raison d'être and only advances in mass spectrometry brought a real breakthrough.

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A novel portable device for fast and sensitive analysis of explosives in environmental samples is presented. The developed system consists of miniaturized microcolumn liquid chromatograph, photolytic converter and chemiluminescence detector. The device is able to determine selectively nitramine- and nitroester- and most of nitroaromates-based explosives as well as inorganic nitrates at trace concentrations in water or soil extracts in less than 8 min.

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Performing gradient liquid chromatography at constant pressure instead of constant flow rate has serious potential for shortening the analysis time and increasing the productivity of HPLC instruments that use gradient methods. However, in the constant pressure mode the decreasing column permeability during a long period of time negatively affects the repeatability of retention time. Thus a volume-based approach, in which the detector signal is plotted as a function of retention volume, must be taken into consideration.

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A simple splitless gradient liquid chromatographic system for micro and nano column separations has been assembled and tested. It consists of an OEM programmable syringe pump equipped with a glass microsyringe and ten-port selector valve. Gradient of mobile phase was created in the syringe barrel due to turbulent mixing.

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