Dear Carlos. I saw your question. I think that H2-TPR technique is better than TPO for measuring OSC of ceria. Because the OSC of ceria will react reductants, such as H2, however, technique of oxidation reation "TPO" will react forward negative or merely. I recommend it. In addition, I also recommend XPS O1s technique. The XPS shows O1s trend and intensity.

Thank you Woojoon. Maybe, I must said TPD-O2, what do you think about?

I am wondering that reacting O2 adsorption on material which is ceria and/or contained ceria. I know that O2-TPD process is, first, must do adsorption O2 on material surface, then confirm O2 desorption trend with increasing temperature. Hmm.. Can O2 reacts oxygen species (OSC) of ceria?

You can do transient tests using CO. You pass CO over the sample which due to the OSC will be converted to CO2, when that CO2 stops being produced and CO breaks through again you know you have consumed all the oxygen stored. If you switch between oxygen and CO environments you can get an idea about the rate of release and regeneration of OSC capacity also, and do it at different isothermal conditions as OSC changes depending on temperature.

I guess cycling or transient TPO is a very good option. You may see some good works from Serafin Bernal group here at Researchgate.