The article describes the synthesis of the new ferrocene-substituted calix[4]arene derivative 4 as sensitive layer, and suggests that the immobilization of it is on a quartz crystal microbalance gold electrode via the drop-casting method in order to produce the calix[4]arene-based QCM sensor. In addition, sensor response of the calix[4]arene-based QCM sensor was investigated towards carbon dioxide (CO2) and carbon monoxide (CO). The sensing and selectivity studies show that the ferrocene-substituted calix[4]arene-based QCM sensor is an effective gas sensor toward both carbon dioxide and carbon monoxide.