A pilot scale vapor permeation unit was assembled to study the dehydration of bioethanols with NaA membrane. The operational parameters, such as feed concentration, temperature, and downstream pressure in permeate, were varied. Long-term operation of an ethanol dehydration unit was demonstrated. Additionally, the lingocellulosic ethanol distillate was dehydrated to fuel grade ethanol with less than 1% water content. The changes in impurities, such as methanol, ethylacetate, 2-propanol, 1-propanol, 1-butanol, and Isoamyl alcohol, were dependent on the volatility of the compounds. The ethanol concentrations in the permeate stream were lower than 1%, indicating high separation performance of the membrane system.