A new method for determining the Ni metal surface area of MgO supported catalysts is proposed. Different series of MgO supported Ni catalysts were prepared and titrated by chemical adsorption of oxygen inside an STA-MS setup. Simultaneous recording of the mass gain upon oxidation, the enthalpy of formation of the oxide and the evolved gas allowed a precise quantification of the metallic Ni surface area. In addition, any uncertainties linked with the complex Ni oxide stoichiometry could be ruled out. A comparison of the newly developed oxygen pulse method with already established techniques using H-2 or N2O confirmed the applicability of the method and further revealed its surface sensitivity and accuracy with respect to MgO supported Ni catalysts.