During the last 10 years, high atmospheric concentrations of airborne particles recorded in the Mexico City metropolitan area have caused concern because of their potential harmful effects on human health. Four monitoring campaigns have been carried out in the Mexico City metropolitan area during 2000-2002 at three sites: (1) Xalostoc, located in an industrial region; (2) La Merced, located in a commercial area; and (3) Pedregal, located in a residential area. Results of gravimetric and chemical analyses of 330 samples of particulate matter (PM) with an aerodynamic diameter less than 2.5 microm (PM2.5) and PM with an aerodynamic diameter less than 10 microm (PM10) indicate that (1) PM2.5/PM10 average ratios were 0.42, 0.46, and 0.52 for Xalostoc, La Merced, and Pedregal, respectively; (2) the highest PM2.5 and PM10 concentrations were found at the industrial site; (3) PM2.5 and PM10 concentrations were lower at nighttime; (4) PM2.5 and PM10 spatial averages concentrations were 35 and 76 microg/m3, respectively; and (5) when the PM2.5 standard was exceeded, nitrate, sulfate, ammonium, organic carbon, and elemental carbon concentrations were high. Twenty-four hour averaged PM2.5 concentrations in Mexico City and Sao Paulo were similar to those recorded in the 1980s in Los Angeles. PM10 concentrations were comparable in Sao Paulo and Mexico City but 3-fold lower than those found in Santiago.