The volatile compounds from ash-leaf maple (Acer negundo L.) were examined by adsorption-thermodesorption and GC-MS. Thirty-two compounds, including alcohols, ketones, aldehydes, esters, terpenoids, carboxylic acids, etc. were identified. The analysis revealed that the diurnal rhythm of release of volatile compounds from maple differed in July and in August. In July, the releasing of most volatile compounds reached the peak at 14 o'clock, when in August, the emission of volatile compounds reached the peak at 10 o'clock. Besides diurnal rhythm, there also existed other differences in the releasing of volatiles and their relative contents in July and in August. A possible explanation for this phenomenon is the maturation of leaves, since the sampling conditions were the same both in July and August. At the same time, the response of Anoplophora glabrpennis Motschulsky to volatiles was examined with field bioassay with traps. cis-3-hexen-1-ol was found to be more effective to attract A. glabrpennis than other volatiles released by ash-leaf maple tree in field trapping test. A mixture of 1-butanol, 1-pentanol and 2-pentanol was tested to be the most attractive to A. glabripennis among all tested volatiles. More field trapping tests should be conducted.