Larger voids in mechanically stable, loose packings of 1.3 μm frictional, cohesive particles: Their reconstruction, statistical analysis, and impact on separation efficiency

• 75 μm i.d. columns are slurry-packed with 1.3 μm frictional, cohesive particles.
• The slurry concentration is increased gradually from 5 to 50 mg/mL.
• Packing microstructure is reconstructed using confocal laser scanning microscopy.
• Increased slurry concentrations suppress transcolumn bed heterogeneities.
• Too concentrated slurries favour the formation of larger voids in the packing.

Lateral transcolumn heterogeneities and the presence of larger voids in a packing (comparable to the particle size) can limit the preparation of efficient chromatographic columns. Optimizing and understanding the packing process provides keys to better packing structures and column performance. Here, we investigate the slurry-packing process for a set of capillary columns packed with C18-modified, 1.3 μm bridged-ethyl hybrid porous silica particles. The slurry concentration used for packing 75 μm i.d. fused-silica capillaries was increased gradually from 5 to 50 mg/mL. An intermediate concentration (20 mg/mL) resulted in the best separation efficiency. Three capillaries from the set representing low, intermediate, and high slurry concentrations were further used for three-dimensional bed reconstruction by confocal laser scanning microscopy and morphological analysis of the bed structure. Previous studies suggest increased slurry concentrations will result in higher column efficiency due to the suppression of transcolumn bed heterogeneities, but only up to a critical concentration. Too concentrated slurries favour the formation of larger packing voids (reaching the size of the average particle diameter). Especially large voids, which can accommodate particles from >90% of the particle size distribution, are responsible for a decrease in column efficiency at high slurry concentrations. Our work illuminates the increasing difficulty of achieving high bed densities with small, frictional, cohesive particles. As particle size decreases interparticle forces become increasingly important and hinder the ease of particle sliding during column packing. While an optimal slurry concentration is identified with respect to bed morphology and separation efficiency under conditions in this work, our results suggest adjustments of this concentration are required with regard to particle size, surface roughness, column dimensions, slurry liquid, and external effects utilized during the packing process (pressure protocol, ultrasound, electric fields).