Experiments were conducted to analyze the concentration of sulfur compounds present in ambient air at the pg or ppt level. The compounds were estimated using GC/PFPD (Gas Chromatography with Pulsed Flame Photometric Detector) analyses with a Thermal Desorber (TD). The analytical results showed very stable and precise retention time values (RSD: < 0.22%), peak area (RSD: < 3.9); the coefficients of the calibration curves were also determined (r²: > 0.991). Also, with respect to the recovery rates of the sulfur compounds from dry air, those for H₂S, MM, DMS and DMDS were 94, 100, 113 and 114%, respectively. In order to evaluate the sulfur chemicals in humid air, a study was conducted at RH of 55 and 100%. The recovery rate at a relative humidity of 55% was similar to that under dry conditions. However, recovery rates of H₂S and MM at RH 100% were reduced to 70 and 77%, respectively.