Dynamic cross-sectional liquid distribution and hold-up in a DN80 separation column filled with structured packings was studied using an ultrafast electron-beam X-ray tomograph with high temporal resolution of 2000 images per second. The modality allows visualisation and characterisation of the counter-current flow before and at the flooding point representing the upper operation limit. Two packings of the same type (Montz B1-MN) with different specific surface area were used to investigate the influence of the packing geometry on the spatial liquid distribution. The system studied was water/air at different gas and liquid loads. The results of the tomographic imaging and corresponding post-processing routines were validated by comparison with conventional draining measurements.