Abstract: The volatile and semi-volatile components of concrete were analyzed by solid phase microextraction gas chromatography-mass spectrometry (SPME-GC/MS).The optimum sampling conditions were investigated including different SPME fibers, equilibrium temperatures and sampling time. The 50/30μm DVB/Carboxen/PDMS fiber showed higher sampling sensitivity at the temperature of 65℃. The sixty-one components were detected, accounting for 89.79% of the total content of the volatile and semi-volatile components. Among them, the content of the twenty-two ester components account for 48.08% as the main source of flavor, the nineteen alkene components for 17.95%, and the thirteen alcoholic components for 23.09%. The relative content of the components including acetic acid, phenyl-methyl ester(14.52%), 3-hexen-1-ol, benzoate(14.11%), 3,7-dimethyl-1,6-octadien-3-ol(13.16%)and α-farnezene(12.66%)is the next. The results suggested that SPME-GC/MS is suitable to analyze concrete rapidly and qualitatively.