A case study to the Xianghai marsh wetlands at downstream of the Huolin river is conducted. Core samples were taken with a gravity corer. Two cores and 78 samples were taken and studied with high-resolution to total sulfur, available sulfur, TOC and pH in different grain size sediments. Results displayed that the high values of total sulfur and available sulfur all existed at granule (silt and clay) in both reed marsh and gleying grassland. Average contents of total sulfur in Xianghai wetlands were close to 700 mg/kg-the average content of total sulfur in world soils. From the top down, contents of total sulfur presented decrease by degrees in different grain size sediments and enriched in the layer of grass roots. Generally speaking, total sulfur and available sulfur increased with TOC.