Immobilization of volative organic compounds (VOCs) in contaminated soils by solidification/stabilization (S/S) processes is an attractive potential remediation process. The objectives of this study were as follows: to evaluate S/S procedures, including a new process with a VOC absorbent and silica coatings; to apply a straightforward and inexpensive analytical technique for characterizing VOC behavior during processing; and to propose the expanded use of waste materials such as contaminated soil, rice hulls, and shredded-tire particles. We investigated how the adsorbents, absorbents and encapsulating agents can be combined to retard volatization and resist acidic aqueous leaching of toluene. The toluene released at each step of the S/S process was determined by an accurate headspace analysis method. Results showed that combining shredded-tire particles for absorption and sodium silicate for encapsulation is a promising method for immobilization of toluene in soil.