The Kelantan River is the main river in Kelantan, Malaysia. It drains along catchment area of approximately 11900 km2 in north-east Malaysia along including part of the Taman Negara National Park, and flows northwards into the South China Sea. The Kelantan River has been used frequently by the local community for domestic uses, transportation, agriculture, plantation irrigation, small scale fishing industries and additionally sand mining activities. The turbidity of Kelantan River is high because of the excessive number of suspended solids and siltation. These have been caused by logging sports within the upstream areas and sand mining sports. The extent of sand mining pastime along the Kelantan River will increase every year because of the high call of sand for enterprise and industry. The aim of this study was to determine the concentration of heavy metals including copper (Cu), aluminium (Al), lead (Pb), zinc (Zn) and iron (Fe) in sediment and to estimate the pollution level of Kelantan River, Kelantan, Malaysia. In research methodology, X-Ray Fluorescence (XRF) test were applied to determine the concentration of each element in the sediment samples. The number of samples tested were 25 and each of them have different concentration of heavy metals. Significant calculations also were done such as Enrichment Factor (EF), Geo-Accumulation Index (Igeo) and Pollution Load Index (PLI) to justify the accuracy of the results. Results indicated that elevated concentrations of Al, Ca, Fe, K and Mn in surface sediments of the study area show significant value as expected based on previous study. The high enrichment factor for K and Mn obtained in the sediment samples show that there is a steady increase of toxic heavy metals risk in this area, which could be correlated with the past mining activity and post abandoned mining in the area.