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Abstract: The acid-volatile sulfide (AVS), simultaneously extracted metals (SEM), total metals, and chemical partitioning in the sediment cores of the Pearl River Estuary (PRE) were studied. The concentrations of total metals, AVS, and SEM in the sediment cores were generally low in the river outlet area, increased along the seaward direction, and decreased again at the seaward boundary of the estuary. The amounts of AVS were generally greater in deeper sediments than in surface sediments. SEM/AVS was >1 in the surface sediments and in the river outlet cores. The ratio was <1 in the sediments down the profiles, suggesting that AVS might play a major role in binding heavy metals in the deep sediments of the PRE. The SEM may contain different chemical forms of trace metals in the sediments, depending on the metal reaction with 1M cold HCl in the AVS procedure compared with the results of the sequential chemical extraction. The SEM/AVS ratio prediction may overestimate trace metal availability even in the sediments with high AVS concentrations. [Copyright &y& Elsevier]