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Synchrotron X-ray absorption spectroscopy (XAS) has become a useful method for the analysis of environmentally relevant elements in natural sediments and soils and in laboratory analog studies. Because of the spectral richness and the ability to analyze different spectral regions by different approaches [X-ray absorption near-edge structure (XANES) vs. extended X-ray absorption fine structure (EXAFS)], XAS provides valuable molecular-scale information on speciation and local bonding. The application of synchrotron XAS to natural materials such as soils, sediments, and biological matter has been increasing in popularity owing to its element specificity, the lack of vacuum requirement, minimal sample preparation, the ability to make bulk or spatially resolved measurements, and the increased accessibility to high-brightness synchrotron beamlines.