This study was performed mainly to examine whether a city with a metal industrial presence presents different characteristics in ambient volatile organic compound (VOC) concentrations compared to residential (RES) and commercial/residential combined (CRC) areas of another city by using long-term monitoring data (from January 2006 to February 2009). For most target VOCs, ambient concentrations in the metal-industrialized city were lower than for the RES and CRC areas. Aromatic compounds were the predominant VOC groups for the metal industry city as well as for other land uses. The ambient concentrations of aromatic VOCs were higher in the winter and spring seasons than in the summer and fall seasons, whereas those of chlorinated VOCs did not show any distinctive variations. In addition, higher concentrations were observed during daytime hours. The correlations between the ambient target compounds were statistically significant, except for the correlation between benzene and ozone.