The diurnal variation of atmospheric carbonyls and VOCs in a forest in south China were studied in summer 2004. Twenty kinds of carbonyls and eight kinds of VOCs were identified and quantified. Formaldehyde and acetaldehyde were the two most abundant carbonyls, while the most abundant VOCs were isoprene, followed by o-xylene. Most C(3)-C(10) carbonyls had higher concentrations from 09:00 to 15:00, and their levels were lower during night-time and often reached the lowest in early morning. Formaldehyde and acetaldehyde, however, showed two high levels in their diurnal patterns partly due to their different sources and sinks. The VOCs had different diurnal patterns compared to most carbonyls. The highest concentrations were observed from 03:00 to 06:00 for 1-butene, from 06:00 to 12:00 for isoprene, and from 12:00 to 15:00 for alpha-pinene. The highest levels for aromatic hydrocarbons occurred during midnight and the lowest in late afternoon. According to the study, emissions from vegetation and photo-oxidation of gas-phase hydrocarbons were the main sources for some carbonyls and VOCs in this region. Other compounds, such as formaldehyde, acetaldehyde and BTEX, showed anthropogenic sources.