This paper analyzes the mass fractions of Ce, Co, Cr, Cs, Eu, Fe, Hf, K, La, Lu, Nd, Rb, Sc, Sm, Ta, Tb, Th, U, Yb and Zn determined from sixty sediment samples obtained from the Lapa Grande de Taquaraçu archaeological site using instrumental neutron activation analysis, INAA. The archaeological site is located in the municipality of Jaboticatubas, about 60 km from Belo Horizonte, Minas Gerais State, Brazil. The dataset was explored by means of cluster analysis, principal component analysis and discriminant analysis. The study showed three different compositional groups related to anthropogenic sediment, fluvial system and oxisols, respectively. The crystalline structure of each group were studied using X-ray diffraction, XRD. [ABSTRACT FROM AUTHOR]