Suspended solids and sediment are important in providing substrates for aquatic plants and microbes and in the fate and transport of essential elements and pollutants. This chapter describes the physico-chemical properties of suspended solids and sediment in Tonle Sap Lake. The solids and sediment consist of clay minerals in the form of smectite and illite. Elemental analysis indicated primarily silicon, aluminum, and iron elements with an average content of 34.3%, 8.3%, and 3.9% in mass ratio, respectively. This result was expected because those elements are the major constituents of the earth’s crust. Moreover, the geo-accumulation index analysis indicated that the pollution of iron from anthropogenic sources is unlikely. However, the high concentration of iron compared to the values in other lakes implies anthropogenic effects. High phosphorus content (up to 14.0%) was detected in sediment in the northern part of the lake, which is attributed to anthropogenic activities. The sediment analysis also indicated a relatively high lead content of 36.7 mg/kg on average. Furthermore, an additional finding of high lead concentration in lake water emphasized a potential risk to humans and the environment; thus, continuous monitoring of lead concentration in lake water and sediment and additional research are necessary.