This study combined different approaches to characterize organic sediments produced by an anaerobic digestion plant feed with pig slurry, and accumulated for many years in a lagoon. The results of all analyses identified a certain homogeneity of the sediments. As a consequence of the pig diet, the sediment contained an high concentration of Zn (about 4 g kg-1) and Cu (about 1.2 g(-1)), which Were mostly associated to the particles with a size ranging from 2 to 53 pm. The sediment was made of large amount of organic matter, mostly cellulose and recalcitrant molecules, and 30-40% mineral fraction. XANES and XES spectroscopies indicated the presence of zinc phosphate (38%), zinc sulfide (32%), zinc carbonate (19%), and zinc oxide (11%). The presence in the sediment of forms characterized by a very scarce solubility, as also confirmed by the Zn and Cu chemical speciation, indicated a low bioavailability of these metals. However, although their low mobility, the high concentrations of Zn and Cu allowed to consider the sediment not suitable to use as a fertiliser due to the potential risk of metal interaction with the food chain. (C) 2017 Elsevier B.V. All rights reserved.