Radioelement contents of rock samples collected from some locations in the Sokoto Basin of Nigeria, where radiometric anomalies had earlier been delineated by gamma-ray spectrometric surveys, were determined by X-ray fluorescence technique using238Pu and109Cd excitation sources. The uranium contents determined were compared with delayed neutron counting results, while flame emission spectrometry was used to cross-check potassium contents. The analyses revealed uranium and thorium enrichments, with U/Th ratio of about 1.8, and negligible potassium concentrations in most samples.