In order to support the tritium production and recycling in the fuel cycle system of fusion reactors, the thermal cycling absorption process (TCAP), which is a semi-continuous chromatographic process for hydrogen isotope separation, has been developed for years. The hydrogen isotopes separation capacity mostly depends on the efficiency of the separation columns, therefore, evaluating different column structure designs and packing materials for their separation efficiency is significative. In this work, a unique design of separation column apparatus with the hot/cold cycling system has been developed. Its unique feature is the different separation columns can be changed for testing several factors such as particle size of packing material, fill density and uniformity, column structure on the influence of the column efficiency. Moreover, the methods to measure efficiency of the separation column have been introduced. The experimental results show that the displacement chromatographic method is more suitable for this apparatus to analyze the column efficiency. Copyright (C) 2014, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.