New high-pressure LC (packed microcapillary) columns are described which consist of small adsorbent particles drawn Inside glass capillaries of 50-200 pm internal diameters. A typical ratio of the column inner diameter to particle size is 2, and a significant plate-height reduction is achieved with decreasing particle size. With typical flow rates of several pL/min through such columns, modlfied injection and detection techniques are necessary. The columns of different inner diameters and particle sizes were evaluated through the reduced plate height vs. velocity plots. The effect of column coiling diameter on chromatographlc performance was also studied. Whereas sample capacity of packed microcapillary columns is low, typical column efficiencies are significantly higher than those obtained with the hitherto available LC c o I u m n s .T h e basic types of columns available in analytical gas chromatography (GC) are conventional packed columns, open tubular (capillary) columns, micropacked columns (with typical internal diameters around 1 mm), and packed capillary columns. These columns differ widely in terms of separation efficiency and sample capacity. Selection of a column type in liquid chromatography (LC) has been more restricted because of viscosities and solute diffusivities in the liquid phase which are orders of magnitude different from the values in the gas phase.T h e most efficient columns presently used in LC are those packed with totally porous small particles (with particle size down to several micrometers). T h e other column types, as known in GC, have not been sufficiently explored. This is primarily due t o t h e fact that the mass transfer is a diffusion-controlled process. Thus, capillary LC is unlikely to give desired efficiencies under t h e conditions of laminar flow.Packed capillary columns studied extensively in GC byHalasz and Heine ( I ) and Landault and Guiochon (2) have rather unique characteristics. Their technology is different from other column types in that t h e adsorptive material is drawn inside the glass capillaries, in a way that is somewhat similar to the very common method for preparation of glass capillary helices (3). However, according to Halasz and Heine ( I ) , t h e most important feature of such columns is the ratio of particle size to the internal column diameter. Whereas packed capillaries possess usual values of this ratio between 0.2 and 0.5, t h e conventional packed columns are typically well below 0.1. Thus, packed capillaries have certain geometrical characteristics of their own which are reflected in their analytical performance. Considering a rather loose packing of these columns used in GC, their efficiencies are quite high. Halasz and Heine ( 1 ) attribute this to the mobile-phase mixing effect that aids the radial diffusion and stress t h e importance of high column permeability.When comparing the theoretical separating power of GC and LC with t h e actual situation, Giddings ( 4 , 5 ) and Golay (6) note that, unlike in GC where a reasonable approach has...