In this paper, the cavity perturbation method was used to measure the dielectric properties of materials that are important for understanding the response to microwave waves, in terms of the ability of these materials to store energy and dissipate it as heat, respectively. Compounds (polyester / walnut shells) were prepared, and for different weight concentrations of walnut shells (WS) additive, the proportions ranged between (0% - 25%). The used cavity is rectangular in shape with a theoretically resonance frequency of around (9.9978 GHz) and exiting the dominant mode (TE101). The study shows the highest values of each dielectric constant with a weight concentration (25%) of the walnut shells, and the loss tangent without any material change to the sample. These compounds have been found to be useful in applications of electromagnetic materials such as microwave engineering and protection from biological influences when exposed to the field of microwaves, which is why it is very important to test their dielectric properties.