A novel plug-and-play setup based on polycapillary X-ray optics enables three-dimensional (3D) confocal X-ray fluorescence (XRF) and X-ray absorption spectroscopy down to 8 × 8 × 11 μm3 (17 keV) at the European Synchrotron Radiation Facility Collaborative Research Group Dutch-Belgian Beamline, BM26A. A complete description and analytical characterization is presented, together with two recently performed experimental cases. In Deep Earth diamond São Luiz-Frankfurt am Main 16, an olivine-rich inclusion was mapped with full 3D XRF elemental imaging. The preliminary tests on Iron Gall ink contained in an historical document, a letter from the court of King Philip II of Spain, reveal both the delicate nature of Iron Gall ink and the lack of Fe-Ni chemical bonding.