Abstract: Research on the separation of the above-mentioned mixture has been made with the purpose of obtaining concentrated formic acid (90% (wt)) and acetic acid (99% (wt)). By employing ethyl acetate as azeotropic agent, the number of theoretical plates in the dehydration column can be reduced. Batchwise distillation under pressure of 28.66kPa was operated with single pass yield of 65% for formic acid and 80% for acetic acid respectively. Through analog computation, the number of theoretical plates has been estimated as well.