The esparto and the diss play a significant role for the sustainable development. This work provides opportunities to develop cost-effective activated carbons from Stipa Tenacissima (Esparto or Alfa is the Arab name for esparto) and diss ( Ampelodesmos mauritanicus). The preparation of activated carbon from agricultural waste could increase economic return and reduce pollution. The objectives of this work are the elaboration and the characterization of activated carbon (ACs) from diss and esparto grass fibres under vacuum condition with chemical activation method using zinc chloride (ZnCl 2 ) as activating agents. The surface organic structures were studied using a FTIR spectroscopy. The surface morphology of the activated carbons was analyzed using a scanning electron microscopy (SEM) and energy dispersive analysis of X-rays (EDX). To define the metallic oxides residues we analyzed the samples by X-ray diffraction (Small-Angle X-ray Scattering). The BET surface areas of the activated carbons from esparto and diss fibres produced are 953m²/g and 754m²/g, respectively. The pore size was calculated by the BJH method. The distribution could be tailored in the range of 1.3-2.7nm. The activated carbons (AC) so developed were able to remove 0.042 mmole/g of Methylene blue (MB). These experimental results indicated the future use of esparto and diss fibres for removing a wide variety of metal ions.