Particulate Matter have propensity to penetrate deep into the lungs, bloodstreams, and brain, making it the most dangerous kind of air pollutants, causing health concerns such as heart attacks and respiratory disorders. Thus, this research is focused on investigating the concentration of Particulate Matter (PM2.5 and PM10) in μg/m3 of Aerosols in some locations in Katsina Metropolis using energy dispersive X-Ray Fluorescence (EDXRF) Analysis. Results obtained reveal that the average PM 2.5 concentration for Katsina Metropolis ranged from 19-67 μg/m3, while the average PM10 concentration ranged from 112-192 μg/m3, revealing that about 80% of the Particulate Matter loads in Katsina is above the WHO recommended limit. The PM2.5/PM10 ratio of Katsina metropolis (0.28) are below the WHO recommendation (0.5-0.8). Lower ratio implies higher PM10, hence, Katsina Metropolitan Area is polluted with PM. Higher limits of Particulate matter in Katsina metropolis could be as a consequence of urbanization and other economic activities without due regulation and the dust particles from the Sahara blowing North to South. Therefore, relevant agencies could periodically access the levels of PM in Katsina State in other to take proactive measures for safeguarding the populace.