Column-in-valve designs to minimize extra-column volumes

We report on the design and performance of in-house built column cartridges that can be directly screwed into the ports of a commercial rotor-stator valve to minimize extra-column band broadening and pressure-drop losses when pursuing ultra-fast separations such as those needed in 2D and 3D-LC separations. Two basic designs were evaluated and were compared with the results obtained with a commercial screw-in column cartridge. The system produces an extra-column band broadening as low as 0.05 to 0.1 mu L 2 for the employed UV-detector set-up. Despite these very low values, the obtained separation efficiency of the in-house fabricated cartridge columns was very low, corresponding to a reduced minimal plate height around h = 7 at the very best, which, for the 1.7 mu m particle and 26.4 mm long columns corresponds to a number of theoretical plates of N = 2200 under isocratic conditions. A similar poor performance was obtained with a commercial column cartridge with similar dimensions using the same set-up. One possible explanation of the observed performance could be found in the inner diameter of the column cartridges (i.d. = 0.75 mm and 1 mm) which, for the employed sub 2 mu m particles, falls into a region of column diameters that, according to literature models, is most likely to suffer from inherent packing problems. (C) 2020 Elsevier B.V. All rights reserved.