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Barrier layers against intermetallic diffusion are a fundamental part on engineering electroplated coatings as they improve the lifetime of goods reducing wastes and improving the sustainability of the production chain. This study aims to set a cost-effective methodology to characterize barrier systems by evaluating the effectiveness with a recent approach based on XRF and EDS and characterize the kinetic of diffusion processes with X-ray diffractometry. Several high fashion barrier systems were tested highlighting that anticorrosion systems are not automatically suited as barrier layers for intermetallic diffusion, as opposed to industrial practice. Investigations on gold coatings obtained varying the current density revealed a correlation between the activation energy of the diffusion process, roughness, and crystallite size.