We investigated the effect of temperature on the packing procedure of nano-LC columns (up to 50 cm) and on their performance. Several slurries of stationary phase were prepared using different solventmixtures. Their stability was evaluated at several temperatures: 70C, 50C, and room temperature. At the higher temperature (70C) the suspensions resulted to be stable for a longer time. For each slurry, we compared nano-LC columns packed with ultrasounds at 70C and at room temperature. All the columns were tested with a standard mixture at 70C, to reduce the solvent viscosity and the backpressure.Main chromatographic parameters such as the asymmetry factor, As, the reduced plate high, h, pattern in a Van Deemter plot, the total porosity, t, and the permeability, k, were calculated and discussed. One of the nano-LC columns was used to separate a mixture of pesticides in a LC-MS system with an electron ionization LC-MS interface (Direct-EI). From our knowledge, this is the first study on the role of temperature in the efficiency of slurry-packing procedure.
Temperature effects on nano-LC column packing technology
LEONARDIS, IRENE;CAPRIOTTI, FABIANA;CAPPIELLO, ACHILLE;FAMIGLINI, GIORGIO;PALMA, PIERANGELA
2012
Abstract
We investigated the effect of temperature on the packing procedure of nano-LC columns (up to 50 cm) and on their performance. Several slurries of stationary phase were prepared using different solventmixtures. Their stability was evaluated at several temperatures: 70C, 50C, and room temperature. At the higher temperature (70C) the suspensions resulted to be stable for a longer time. For each slurry, we compared nano-LC columns packed with ultrasounds at 70C and at room temperature. All the columns were tested with a standard mixture at 70C, to reduce the solvent viscosity and the backpressure.Main chromatographic parameters such as the asymmetry factor, As, the reduced plate high, h, pattern in a Van Deemter plot, the total porosity, t, and the permeability, k, were calculated and discussed. One of the nano-LC columns was used to separate a mixture of pesticides in a LC-MS system with an electron ionization LC-MS interface (Direct-EI). From our knowledge, this is the first study on the role of temperature in the efficiency of slurry-packing procedure.I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
