A novel method was devel- oped for the selective determina- tion of lead (Pb) in environ- mental samples by displacement dispersive liquid-liquid microex- traction (D-DLLME) combined with graphite furnace atomic absorption spectrometry (GFAAS). This D-DLLME method involves two steps of dispersive liquid-liquid microextraction (DLLME). Firstly, Zn2+ reacted with diethyldithiocarbamate (DDTC) to form the Zn-DDTC complex and was then extracted with the DLLME procedure. Then the sediment phase was dispersed into the sample solution contain- ing Pb2+ with a dispersive sol- vent; then another DLLME procedure was carried out. Since the stability of Pb-DDTC is higher than that of Zn-DDTC, Pb2+ can displace Zn2+ from the pre- extracted Zn-DDTC complex and be preconcentrated into the sedi- ment phase. The interference from co-existing metal ions with a lower DDTC complex stability was largely eliminated as they cannot displace Zn2+ from the Zn-DDTC complex. Under the optimal conditions, the limit of detection was 35 ng L?1 (3σ) for lead, and an enhancement factor of 91 was achieved with a sample volume of 5.0 mL. The proposed method has been successfully applied to the determination of trace lead in environmental sam- ples with satisfactory results.