The analysis of individual micrometre- and submicrometre-sized particles collected by IAEA’s safeguards inspectors on swipe samples during in-field verification activities requires the implementation of a sustainable quality control system such as suitable microparticulate reference materials. To this end, pure and neodymium-doped uranium oxide-based microparticles utilising an aerosol-based particle production process were prepared. SEM/EDX measurements confirmed the monodispersity of the produced microspheres as well as the incorporation of 15 mol% Nd into the compound particles. The timeline of structural investigations mirror the ongoing alteration of particles being stored under laboratory atmosphere. While results from in-SEM Raman (CEA, DAM) on microparticles after two years storage time point to the formation of U3O8 and a minor fraction of schoepite phase (hydrated UO3), in U L3-edge XAFS after four months storage time and U M4-edge HR-XANES after ten months storage time spectra (INE-Beamline and ACT station @ KIT synchrotron radiation source) mainly U(IV) and U(V), respectively, was observed. These results provide new insight into ageing mechanism of the microparticles after preparation. ... mehrFrom these results important conclusions with respect to storage conditions and shelf life of the reference particles can be drawn. The first batch of pure U-oxide microparticles produced in Juelich was successfully certified regarding the isotopic composition and the U amount per particle and applied in an international laboratory exercise NUSIMEP-9.