Metallic surface of Cu/ZSM-5 catalyst was determined quantitatively with H 2 TPD and N 2O oxidation methods. Usually well established N 2O techniques are the dissociative N 2O chemisorption performed as pulse chemisorption or in frontal technique with highly diluted N 2O to avoid high heat evolution and bulk oxidation. Here TPR/H 2 of the oxygen layer formed under relatively high N 2O partial pressure is compared with TPD/H 2. The dispersion of Cu 0 determined by TPD is very high. The calculated metallic surface copper area was very close to the total exchanged Cu in the sample, which confirms that copper atoms are well dispersed on ZSM-5 sample. These measurements are supported by XPS data, suggesting also a high dispersion of copper ions in the zeolite. The surface metallic copper determined by H 2 TPD technique showed that this method avoids sintering, compared to the N 2O method, where sintering occurred due to heat evolution during the N 2O reaction, causing migration and agglomeration of copper externally the surface of the zeolite.