Resistant desorption has been widely observed for hydrophobic organic contaminants. It is an important process that impacts sediment quality and contaminated sediment management. Conventional approaches to measure the desorption resistant fraction of sorbed contaminants are by conducting repetitive water desorption, in which the desorption resistant fraction is determined by measuring the solid phase concentration after extended desorption times. This method is time-consuming and impractical for widespread applications. In addition, the final measurement of the solid phase concentration is subject to considerable error, because there is always a fraction of water associated with the solid due to the incomplete separation of the liquid phase from the solid. In this research, a new experimental protocol was developed to rapidly and accurately measure the desorption resistant fraction based on the study of desorption of phenanthrene from Utica sediment.