Micro-residue analysis of stone tools is generally performed with optical light microscopy and the visual observations are then compared with experimental, replicated pieces. This paper complements such archaeological research by providing physico-chemical evidence. Raman spectroscopy and scanning electron microscopy have been used to confirm the presence of hematite on red-stained medial and proximal parts of 71 000-year-old Still Bay bifacial tools from Sibudu Cave. Our results confirm the conclusion from optical light microscopy that the tools were hafted with an ochre-loaded adhesive. However, we point to some instances when hematite residues are incidental or may be inclusions in the rock used to make the stone tools.