This study was undertaken to investigate the heavy metals pollution in the Great Usuthu River (Swaziland). The influence of major pollution sites were assessed using chemometric methods, namely cluster and discrimination analyses. Levels of lead, chromium, vanadium, cadmium and cobalt were determined in both water and sediment samples. In addition chemical oxygen demand was also determined for the water samples. The statistical methods indicated the major parameters discriminating the sampling sites characteristics and showed the seasonality in the dataset.