Heat transfer and kinetic parameters of wall-cooled fixed-bed reactors are traditionally obtained through separate heat transfer and kinetic experiments. In spite of its simplicity, the uncertainties resulting from the low parametric sensitivity and high correlationship among the parameters inevitably make the estimation unsuitable for safe extension to actual reacting conditions. In this paper, an effort was made to estimate simultaneously both heat transfer and kinetic parameters under reacting conditions in a single tube wall-cooled fixed-bed reactor, and a two-stage parameter estimation procedure was developed. The correlation and confidence region analysis performed in this paper verifies both theoretical and experimental feasibility of simultaneous estimation of heat transfer and kinetic parameters under real reacting conditions.