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In the archaeometallurgical study of iron nails to investigate Roman manufacturing processes, multi-analyte characterization provides information on alloy composition and microstructure. Nails from the Roman sites of Forua, Aloria, and Iuliobriga (northern Spain) were studied. To characterize the iron phases and microstructures of the nails, optical microscopy (OM), scanning electron microscopy coupled with electron-dispersive spectroscopy (SEM-EDX), micro-Raman spectroscopy, electron backscatter diffraction (EBSD) realized in environmental mode, and microhardness measurements were carried out. The chemical composition of the metal was determined by X-ray fluorescence (XRF). The corrosion mineralogical composition was determined by powder X-ray diffraction (XRD). Aggressive burial conditions had a significant effect on the forms of corrosion of the Forua nails to the point of complete iron loss. Examination of the metal of the nails from the Aloria site revealed that most of the ironwork was made in the villa’s own forge. In the case of the Iuliobriga nails, different degrees of forging were identified associated with different workshops.
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