Volcanic tuff and walnut shells were tested as natural adsorbents materials for the removal of Pb(II) and As(V) from waste water. Inductively coupled plasma mass spectrometer (ICP-MS) and an atomic absorption spectrometer were used to monitor the concentration of metal ions in aqueous systems. The sorption capacity of these adsorbents were evaluated at different experimental conditions. The effect of time, initial concentration of the metals and the adsorbent dose on the adsorption was studied. The lead removal efficiency using volcanic tuff at pH value of 4 was more than 99 % in all concentration range investigated, while in the case walnut shells at pH value of 2, the maximum efficiency was 53.2%. Regarding the arsenic uptake at low concentration, the best performance was registered for walnut shells (50.15%). The two low-cost natural sorbents were efficient to remove both pollutants from aqueous systems and may be considered as a viable alternative to conventional adsorbents.