Rapid industrialization over the past century has led to increased irresponsible resource extraction, exacerbating environmental contamination globally. Industrial activities contribute significantly to the accumulation of heavy metals in water and sediment, which is further intensified by accelerating industrialization. Concerns about the environmental and health impacts of heavy metals such as cadmium (Cd), lead (Pb), copper (Cu), nickel (Ni), and zinc (Zn) have grown, emphasising the need for comprehensive analyses. Sungai Gemang, situated near the community of Kampung Gemang, serves as a vital water and protein source for the nearby population. Due to the potential carcinogenic and toxic nature of some metal contaminants, their impact on both the environment and human health warrants investigation. This study aims to determine the concentrations of heavy metals (Pb, Cd, Cu, Zn, and Ni) in both sediment and water in Sungai Gemang, Jeli, and Kelantan. Additionally, it seeks to establish correlations between metal concentrations in sediment and water bodies. The methodology involves the collection of 3 samples of water and sediment samples at three sampling stations from Sungai Gemang, followed by an acid digestion method to digest the samples for analysis using atomic absorption spectroscopy (AAS). Risk characterization is performed through the application of Sediment Quality Guidelines (SQG), Geoaccumulation Index (Igeo), and Enrichment Factor (EF). The results indicate a low distribution of metal concentrations in Sungai Gemang, suggesting an uncontaminated status of the water sources. While water quality meets acceptable standards, the elevated metal concentrations in sediment compared to water highlight the dynamic interplay between water and sediment, emphasising the importance of sustainable management practices for this crucial aquatic ecosystem.