Bituminous sands from south-western Nigeria were separated into water and sand fractions, and these were analysed for their physico-chemical properties and trace-metal contents to evaluate their potential environmental hazards. The samples were obtained from five different locations (Ilubirin, Agbabu, Mile 2, Olowo-Irele, and Loda) in Ondo State, south-western Nigeria. The water content was extracted using Dean and Stark apparatus, while the sands were collected as left-over from the thimble. The trace metal content was determined using total X-ray fluorescence (TXRF) spectrometry. The physico-chemical parameters (conductivity, pH, total alkalinity, total acidity, salinity, colour, organic matter, Cl⁻, , and ) were determined using standard analytical methods. Copper, Cr, Zn, and As, which are known to be toxic metals, were highly enriched (enrichment factor, EF>10) in the sand fraction samples, while comparison of some of the physico-chemical parameter values of the water and sand fractions with recommended standards showed that the values of some of the parameters were relatively high. These values indicate their potential environmental hazards. This calls for proper management of the tailings that will be produced during the exploitation of the bituminous sands. Analysis of certified IAEA standard reference material (IAEA-soil-7) was carried out to ensure accuracy and precision of the TXRF technique.