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Abstract.New adsorbents PAMAM-n.0TMSG (n=1,2,3,4) with thiomalic acid as functional group has been prepared based on polyamidoamine dendrimer modified silica gel and characterized with FTIR, SEM and TG. Microcolumn enrichment and measurement of Pb 2+ with graphite furnace atomic absorption spectroscopy (GFAAS) was investigated with PAMAM-n.0TMSG (n=1,2,3,4) as adsorbent. The adsorption conditions were optimized. The increase of grafted generation of PAMAM-n.0TMSG could effectively improved the adsorption performance of adsorbents. The adsorption capacity of adsorbents was 14. 42, 16.19, 20.79 and 25.32 mg g -1 respectively, With PAMAM-4.0TMSG as adsorbent, microcolumn enrichment and measurement of Pb 2+ with GFAAS was proposed. The relative standard deviation (R.S.D.) was 1.4% (n=11) for 0.2 μg mL -1 of Pb 2+. The limit of detection (LOD) of 2.9ng mL í1 was achieved. The proposed column enrichment method was applied for detection of Pb 2+ in tap water and sea water samples successfully.