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The adsorption of Cu(Ⅱ) and Cr(Ⅵ) on diaspore was studied with the help of X-ray diffraction analysis, BET measurement, zeta potential measurement and atomic adsorption spectrometry. The adsorption equilibrium almost reaches within 60 min. The adsorption isotherms of Cu(Ⅱ) and Cr(Ⅵ) could be well described by the Langmuir equation. The adsorption capacities of Cu(Ⅱ) and Cr(Ⅵ) are 1.944 and 1.292 mg/g, respectively. The adsorption percentage of Cr(Ⅱ) increases with the increment of solution pH, but the adsorption percentage of Cr(Ⅵ) decreases. This could be explained by zeta potential theoretical and electrostatic attraction between metal ions and diaspore surface.