The adverse health effects of airborne particles have been subjected to intense investigation in recent years; however, more studies on the chemical characterization of particles from pollution emissions are needed to (1) identify emission sources, (2) better understand the relative toxicity of particles, and (3) pinpoint more targeted emission control strategies and regulations. The main objective of this study was to assess the levels and spatial distribution of airborne chemical elements in a heavy industrial area located in the north of Spain. Instrumental and biomonitoring techniques were integrated and analytical methods for k0 instrumental neutron activation analysis and particle-induced x-ray emission were used to determine element content in aerosol filters and lichens. Results indicated that in general local industry contributed to the emissions of As, Sb, Cu, V, and Ni, which are associated with combustion processes. In addition, the steelwork emitted significant quantities of Fe and Mn and the cement factory was associated with Ca emissions. The spatial distribution of Zn and Al also indicated an important contribution of two industries located outside the studied area.