Failures caused by carbon deposits have always been a challenge in hydrocarbon processes. In this paper, a nonlinear acoustic resonance technique was investigated to characterize heterogeneous deposits on the surface of metal structures. The amplitudefrequency curves of the fundamental and secondharmonic responses were measured at various excitation levels. Experimental results indicated that the dependence of the resonant spectrum of the second harmonic response on the excitation level is based on the status of the deposit. Moreover, two hysteretic nonlinear parameters related to the second harmonic, the hysteretic elastic nonlinearity and the hysteretic dissipative nonlinearity, were proposed for the quantitative characterization of the deposited layers. The developed nonlinear acoustic resonance method in the megahertz region was used for quantitative evaluation of carbon deposits in a pipe, and the feasibility of the method for assessing carbon deposits was demonstrated.