Approximately 50 mg of dried and pulverized sediments underwent total digestion by using 1.5 ml high purity HNO3 and 1.5 ml HF in a microwave oven for 48 h at 190 C. And then 1 ml HNO3 was added to the residue on the hot plate to remove the remnant HF. The residue was solubilized by 3 ml HNO3 and kept in the oven for 8 h at 150 C. The heavy metal (Cu, Pb, Zn, Cr, and Cd) contents were measured by ICP-MS (X Series 2) after the extracting solution was diluted to 50 mL volume with deionized water. The standard reference materials (GSD-9, stream sediments) were analyzed as control samples for quality assurance. The recoveries of GSD-9 ranged from 95% to 105%. Grain size, clay minerals, and elemental analyses were done in the Key Laboratory of Marine Sedimentology and Environmental Geology, State Oceanic Administration, China.