A new grapheme oxide/thiacalixarene composites material was synthesized.The characterization of this material was performed by SEM，FT-IR，Element analysis and thermal analysis.A new method for the determinaon of trace thallium was developed by graphite furnace atomic absorption spectrometry（GFAAS） with the grapheme oxide/thiacalixarene composites material as adsorbent.The optimal experimental conditions（e.g.pH value of solution，temperature，elution condition） and the adsorbing principle for the determination were studied.It was found that thallium could be adsorbed on grapheme oxide/thiacalixarene composites material at pH 8.0 and temperature of （23±1）℃，and the adsorption capacity was 73.1 mg/g.The determination of trace thallium was performed by GFAAS after it was eluted with 5 mL 0.5 mol/L HCl-1.0 mol/L thiurea.The linear range of thallium ranged from 0.012 μg/L to 15 μg/L.The detection limit（3σ）was 0.008 g/L.The RSD（n=7） for 0.50 μg/L Tl3+ standard solution was 2.3%.The spiked recoveries of thallium were in the range of 93.6%-104.1%.The method was applied in the determination of trace thallium in environmental samples with satisfactory results.