RESUMO
Simulating polymer separation in flow-through channels of monolithic columns, separation of a mixture of polystyrene standards was investigated using open tubular capillary column of 2 µm inner diameter. High column efficiency was observed for polymers of molar mass ranged from few tens to few hundred kDas. Column efficiency significantly decreased for polymers with molar mass larger than 500 kDa nevertheless preserving value of few tens of thousands theoretical plates. Calibration curve observed for open capillary column is rather steep and can be well described by simple equation without quadratic term. In spite of low selectivity, capillary columns were able in separating wide range of polystyrene standards due to column high efficiency and in such a way supported an idea of hydrodynamic mechanism of polymer separation in flow-through channel of monolithic packings.
RESUMO
Low capacity anion exchangers for IC have been prepared by modification of nonporous uniformed silica MICRA microbeads and by modification of the organic polymeric monolithic matrixes prepared in situ in quarz capillary. Due to the small particle size (1.5 microm) high-performance adsorbents were prepared allowing to obtain up to 190,000 tp/m. However, the column possesses a very high back-pressure and can be used in a short length up to 50 mm only to meet the requirements of conventional chromatographic equipment. An analysis of a test mixture of seven anions was completed within 3 min with a back column pressure of about 350 bar (HETP of about 5.5 microm, where HETP is the height equivalent to the theoretical plate). Monolithic capillary columns provide lower efficiency per column unit length than MICRA columns; however, they can be used at a longer length because of their low flow resistance. Monolithic column of ca. 40 cm length has workable pressure below 10 bar and allows separation of a five anions test mixture within less than 10 min. A better efficiency of monolithic column (HETP approximately 75 microm) can be achieved at reduced flow rates when the analysis time is not a critical parameter.
