Abstract：A new extraction separation method of trace thallium（Ⅲ） by microcrystalline naphthalene was studied. The results showed that, in phosphoric acid medium and in presence of 3.0 g of trisodium citrate, when 1.0 mL of 50 μg/mL KBr solution,1.4 mL of 1.0×10-3 mol/L rhodamine B solution and 3.0 mL of 1.0×10-2 mol/L microcrystalline naphthalene propanol solution were selected, the TlBr-4 formed from thallium（Ⅲ） and Br- could react with rhodamine B to form complex, which was quantitatively adsorbed by microcrystalline naphthalene. Under the experimental conditions, other elements such as Al（Ⅲ）, Cu（Ⅱ）, Zn（Ⅱ）, Ni（Ⅱ）, Mn（Ⅱ）, Mg（Ⅱ）, Hg（Ⅱ）, Cr（Ⅲ） and Bi（Ⅲ） were not adsorbed. Based on this, a new separation and enrichment method of thallium（Ⅲ） was established. The proposed method was applied to the separation and determination of thallium in synthetic water samples,and the results were satisfactory.
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