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Precise control and characterization of nanomaterials at working conditions are essential for further rational applications in many areas important for modern society. Penetrating properties of X-ray radiation in combination with advanced spectroscopy schemes are an ideal tool to investigate modifications of nanomaterials with extraordinary precision. Here, we present preliminary results on the controlled oxidation of copper nanoparticles and exploration of X-ray absorption spectroscopy to follow electronic and structural changes. The described pilot experiment raises questions on the applicability of high energy resolution X-ray detection schemes in potential future investigations aimed at following reversible reduction/oxidation processes at nanoparticle surfaces. [ABSTRACT FROM AUTHOR]