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Excavation in the Gnezdovo settlement’s floodplain area has provided evidence of continuous metalworking. Gnezdovo archaeological complex (late IX – early XI centuries) is situated at the Western Russian border at about 13 km from one of the most ancient Russian town Smolensk. It is known as one of the largest archaeological site of the period of State formation in the Eastern Europe. The abundance of slags, fragments of melting pots and shell moulds, handicraft tools, workshop waste in the excavated area are indicative of smithing and silverworking activity. The archaeological study of the area has shown that certain heterochronous structures followed an established pattern, thus being part of a constantly renovated production complex. The workshop existed approximately from 925 to 1000 A.D. Initially the slag samples were identified as smithing hearth bottoms and furnace lining’s fragments. But a recent study of the entire slag collection has shown that some specimens could be interpreted as ore fragments or metallurgical slags. Samples have been investigated using X-ray fluorescence spectroscopy (XRF) and scanning electron microscopy (SEM)to characterize their microstructure and determine their elemental and mineral composition. This paper presents results of the preliminary study of such slags