In this study, the recovery rate of thermal desorbing (TD) method was investigated in relation to sample concentration and loading volume of reduced sulfur compounds (RSC). All the analysis of RSC was made by gas chromatography/pulsed flame photometric detector (GC/PFPD) combined with air server/thermal desorber (AS/TD). The RSC measurement data were obtained by loading gaseous RSC standards prepared at 4 concentrations (10, 20, 50, 100 ppb) at 6 injection volumes (40, 80, 200, 400, 800, and 1200 mL). The recovery rates of each RSC were computed in terms of relationship between expected vs. measured values. According to our analysis, the following conclusions can be drawn. First, the results were less stable at short loading time (1 and 2 min at 40 mL/min) with reduced recovery rate, especially with light RSCs (H₂S and CH₃SH). On the other hand, at sufficiently high loading volume, their quantification was limited by off-scale peaks (at a near 50 ng) due to the breakthrough of cold trap in TD. Thus, the optimization of TD-based analysis may be considered as a prerequisite for analyzing the RSC in a reliable manner.