This research delves into ancient pigment practices among the Goya‐Malabrigo societies in the Upper Delta of the Paraná River during the Late Holocene. Utilising Raman microspectroscopy and X‐ray diffraction, we analysed 33 samples from six archaeological sites and four natural outcrops. Our discoveries uncovered hematite in red pigments across diverse materials (potsherds, shells, human bones, and sediments), anatase adorning ceramics with whitish tones, and charcoal creating darker shades. These findings not only contribute to the understanding of the mineral composition of ancient colours used by Indigenous people in domestic and funerary contexts but also set the first stage for forthcoming provenance research, integrating multiple archaeometric techniques to unravel the origins of these compelling pigments.