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The Ndalambiri rock shelter in the Ebo region of Angola is a key site for assessing human occupation there given its potential association between stratigraphic contexts and rock art panels. Focusing on the Iron Age and European contact periods, this study characterised the site’s rock paintings using Raman spectroscopy, while also obtaining AMS radiocarbon dates from paint residues and charcoal collected in stratigraphic context during a trial excavation below one of the painted panels. Raman spectroscopy results revealed the use of a carbon-based pigment (charcoal?), haematite and calcite to prepare black, red and white paints respectively. AMS dating of a black paint sample showed that it was produced between the seventeenth and the twentieth centuries, corresponding to the last known phase of rock art production in the area, as further indicated by its stratigraphic position and the depiction of firearms at the site. Earlier occupation of the site associated with metallurgical activity was dated to the mid-first millennium AD and may suggest that the oldest rock art at Ndalambiri corresponds to the arrival of metal-using populations in the region. [ABSTRACT FROM AUTHOR]