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Carbonaceous microspheres adsorbents prepared from the carbonisation process of glucose during hydrothermal treatment have been studied for Cr (VI) and phenol removal from aqueous solutions. Carbonaceous microspheres were characterised by scanning electron microscopy, energy-dispersive X-ray analysis and Fourier transform infrared spectroscopies. It was found that there were abundant oxygen-containing functional groups on the surface of the carbonaceous microspheres. The equilibrium data of the adsorption and the effect of pH, initial concentration of pollutant and temperature of solution on the adsorption of Cr (VI) and phenol by carbonaceous microspheres were studied. The carbonaceous microspheres exhibited excellent adsorption capacity for Cr (VI) and phenol.