Abstract: Determination of Fe, Mn, Pb, Zn, Cr and Cu concentrations in Asa River water is discussed. Two different methods of analysis are compared. Atomic Absorption Spectrophotometry (AAS) and X-ray fluorescence (XRF) were employed. A statistical analysis carried out showed that there was no significant difference in the concentrations of Cr, Zn, Pb and Cu using the two techniques. Significant differences were observed at 5% probability level for Mn and Fe using the two techniques. This has been attributed to differences in sample preparation as the two metals have been observed to be mainly of natural origin. It is suggested that they could have been trapped in the micro particles in water since no digestion was carried out prior to XRF analysis.