Volatile species of Cu, Au and Tl were generated at room temperature by the reduction of NaBH4 in acidified aqueous medium using a flow injection vapor generation atomic absorption spectrometric (FI-VGAAS) system. 1, 10-phenanthroline, sodium diethanlydithiocarbonate (DDTC) and palladium (or combined with Rodamne B) ware used as enhancement reagents respectively. The normal flow injection peak shape wase obtained and the sensitivity were enhanced by 1-2 magnitude. The detection limits of 0.34-24ng/ml (3σ) were obtained with 300 or 500µl sample solution. The precision of 2.6-1.8% RSD were obtained with the sampling frequencies were of 120-180/h. The FI-VGAAS methods were used for the determination of copper in hair and rice sample and gold in the ore sample digests.