The characterization of the interface polymer/solid is studied by 1H and 13C NMR. One of the main objectives of this work is to determine the disposition of monomer units near the surface and their concentration. Utilization of different techniques such as multipulse sequences, MAS with variable temperature, observation of the relaxation function of different nuclei, Cross polarisation, allow to propose some approach methodology. The example chosen to illustrate the techniques is the poly (ethylene) oxide grafted on silica. A coherent agreement is obtained for the physical parameter which describes the monomer unit concentration on the surface, by two independent techniques namely pseudo-solid echo and MAS, taking into account the molecular weight and the temperature as pertinent parameters.