Air pollution caused by fine particles is a problem of great concern in the Monterrey Metropolitan Area (MMA) which is the third largest city and the second most important industrial center in Mexico. In this study, samples of fine particulate matter emissions with an aerodynamic diameter of less than 2.5 μm (PM_2.5) were collected for 12-hour periods during the spring and fall of 2011 and 2012. Eighty-three samples were analyzed for organic carbon (OC) and elemental carbon (EC). The carbonaceous fraction (OC + EC) accounted for 28–55% of the PM_2.5 mass. The average OC/EC ratios ranged from 7.4 to 12.6, and OC and EC concentrations were statistically significant correlated (R² = 0.81, p < 0.01). The secondary organic aerosol (SOA) contributions were determined using two approaches: the EC tracer method based on a primary OC/EC ratio derived from a tunnel study and the minimum observed OC/EC ratio. SOAs were determined to constitute, on average, 59–87% and 32–45% of the total OC and PM_2.5, respectively. The relationship between O₃ and wind speed indicated that pollutant levels were influenced by transport events during the spring, while stagnation events predominated during the fall campaigns. Statistically significant correlations were observed between OC and EC and gaseous species (CO, NO_x, and SO₂), indicating a contribution by combustion of fossil fuels to the carbonaceous material.