Platinum/charcoal and nickel/chromium oxide catalysts for the isotopic exchange of deuterium between hydrogen and water vapour were prepared under optimum experimental conditions. The catalytic activity determination of both indicated higher activity for Pt/charcoal than for Ni/Cr2O3. BET measurements of the specific surface area and pore structure showed higher values for Pt/charcoal than for Ni/chromia. Chemisorption data of both catalysts allowed the determination of the specific metallic surface area, the degree of dispersion and the average particle size of the supported metals. A comparison between the results of the catalytic activity, BET measurements and chemisorption was made and indicated close agreement.