The objective of this study was to compare the enrichment performanc of polystyrene-dithizone (PS-DZ) electrospun nanofibrous membrane with commercial cellulose acetate (CA) film for lead in air. Lead was analyzed by preconcentration on different membranes followed by digestion and analysis by Atomic Fluorescence Spectrometry. In comparison to CA film, the PS-DZ electrospun nanofibrous membrane exhibited a significant advantage in enrichment efficiency (about threefold increase). The result confirms that electrospun nanofibrous membrane can be a potential candidate for the sampling of metals in air.