Optimization of post-column reactor radius in capillary high performance liquid chromatography - Effect of chromatographic column diameter and particle diameter

摘要

A post-column reactor consisting of a simple open tube (Capillary Taylor Reactor) affects the performance of a capillary LC in two ways: stealing pressure from the column and adding band spreading. The former is a problem for very small radius reactors, while the latter shows itself for large reactor diameters. We derived an equation that defines the observed number of theoretical plates (Nob,) taking into account the two effects stated above. Making some assumptions and asserting certain conditions led to a final equation with a limited number of variables, namely chromatographic column radius, reactor radius and chromatographic particle diameter. The assumptions and conditions are that the van Deemter equation applies, the mass transfer limitation is for intraparticle diffusion in spherical particles, the velocity is at the optimum, the analyte's retention factor, k', is zero, the post-column reactor is only long enough to allow complete mixing of reagents and analytes and the maximum operating pressure of the pumping system is used. Optimal ranges of the reactor radius (a,) are obtained by comparing the number of observed theoretical plates (and theoretical plates per time) with and without a reactor. Results show that the acceptable reactor radii depend on column diameter, particle diameter, and maximum available pressure. Optimal ranges of a, become narrower as column diameter increases, particle diameter decreases or the maximum pressure is decreased. When the available pressure is 4000 psi, a Capillary Taylor Reactor with 12 mu radius is suitable for all columns smaller than 150 mu m (radius) packed with 2-5 mu m particles. For 1 mu m packing particles, only columns smaller than 42.5 mu m (radius) can be used and the reactor radius needs to be 5 mu m. (c) 2006 Elsevier B.V. All rights reserved.