The storage ring upgrade of the European Synchrotron Radiation Facility makes ESRF–EBS the most brilliant high-energy fourth-generation light source, enabling in situ studies with unprecedented time resolution. While radiation damage is commonly associated with degradation of organic matter such as ionic liquids or polymers in the synchrotron beam, this study clearly shows that highly brilliant X-ray beams readily induce structural changes and beam damage in inorganic matter, too. Here, the reduction of Fe³⁺ to Fe²⁺ in iron oxide nanoparticles by radicals in the brilliant ESRF–EBS beam, not observed before the upgrade, is reported. Radicals are created due to radiolysis of an EtOH–H₂O mixture with low EtOH concentration (∼6 vol%). In light of extended irradiation times during insitu experiments in, for example, battery and catalysis research, beam-induced redox chemistry needs to be understood for proper interpretation of insitu data.