The separation and purification of TaCl5 is indispensable in the synthetic process of TaCl5 by chlorination of tantalum oxide. The reaction products are mainly TaCl5, NbCl5, TiCl4 and FeCl2. However, we need to separate TaCl5/NbCl5 mixture from the reaction product, because TaCl5 and NbCl5 are easily separated each other by distillation or hydrogen reduction process. In this work, a comparison study was carried out between direct sequence and indirect sequence to obtain TaCl5/NbCl5 mixture from the reaction product by removing light component, TiCl4 and heavy component, FeCl2 using two distillation columns. It was concluded that the direct sequence gave better results than indirect sequence in the aspect of initial capital costs and the associative operating costs.