This study concentrates on the environmental pollution level of sediments in the six branches of Poyang Lake, the biggest fresh water lake in China. This is the first systematic report on the speciation analysis of heavy metals (Cu, Co, Cd, Pb, and Ni) in the six branches of the lake. A reported analytical procedure involving a five-step sequential extraction is used for the partition of particulating heavy metals. The sediment samples are analyzed using flame atomic absorption spectroscopy (FAAS). Experimental results obtained from five replicate samples of fluvial bottom surface sediments at the sampling points demonstrated that the relative standard deviation of the sequential extraction procedure was generally better than 10% (Cd except). The average extracted contents of the five elements, analyzed after all five steps, are found to be (mg/kg) for Cu: 26.89, Co: 16.25, Cd: 1.08, Pb: 37.98, and Ni: 20.46. The content of the exchangeable species was generally lower. Except Cu, the percentage of the species bond to organic matter was lower than 20%. The fractions containing the most metal for Cu, Co, and Ni were the residues (52.26%, 45.28%, and 74.82%, respectively).