Abstract: GC-MS method combined with headspace solid phase micro-extraction was used to analyzed the volatile components of wet rubber clots which were prepared by different coagulation ways. There was a difference between the volatile components of the wet rubber clots. The volatile components of biological coagulation gelling block contained more indole, 3-methylindole and phenol, which might cause that biological coagulation gelling block odorous heavier than acid coagulation gelling block.