In this work, the effect of vapor load and initial feed concentrations on column efficiency and liquid hold-up in a two- and three-phase packed distillation column at total reflux was investigated. Results for the two investigated mixtures (n-heptane, n-hexane, water) and (ethyl acetate, 1-butanol, water) reveal that column efficiency remains almost constant for the former mixture but changes significantly for the latter. Specific liquid hold-up and water to organic-phase volumetric ratio within the column affect the column efficiency due to variations in initial feed concentrations. Influence of vapor load on separation efficiency and specific liquid hold-up is also studied.