At Cova Eirós, we discovered 13 panels with paintings and engravings that stylistically point to the final moments of the Upper Paleolithic. Scanning electron microscopy with energy dispersive X-ray spectroscopy and Fourier transform Raman spectroscopy were used to identify charcoal as black pigment. Although contamination from medieval fires inside the cave complicates the dating of these pictographs, analyses of unpainted rock backgrounds allowed calculation corrections for contaminated samples. We used plasma oxidation and accelerator mass spectrometry (AMS) to directly radiocarbon (14C) date two charcoal paintings—confirming that the images are more than 9000 yr old. As these paintings superimpose engravings, these 14C dates also provide a minimum age for an engraving at Cova Eirós that is stylistically Final Magdalenian/Epipaleolithic. This is the first known evidence of Paleolithic cave art in Galicia of NW Iberia.