Batch distillation is becoming increasingly important as a result of the expansion in the fine chemical and pharmaceutical industries characterized by small amounts of the products with high added value. This thesis aimed at finding optimal way of operating batch distillation column using PC-based.The operation strategies for batch distillation were studied methanol and water mixtures with a constant heat duty of 288 W At the beginning of the batch operation, total reflux policy is required. The duration of the total reflux period was chosen as follows: when the distillate temperature (i.e., composition) reached the desired value. The initial volume of the mixture was 1L and all the experiment feed mixture (methanol-water) have the same initial composition, 25%mole of methanol and 75%mole of water. The column works at atmospheric pressure with 10 trays. Batch distillation was operated by using LabVIEW program, the major findings were data acquisition device (DAQ) NI-ELVIS II for acquiring temperatures and generate signals for control purposes...