We analyzed volatile organic compounds (VOCs) of petroleum-based laundry solvents in closed systems by static headspace analysis and investigated the emission characteristics of odorous compounds emitted from organic solvents in the small-scale dry cleaning process. The compounds containing eight to eleven carbon atoms were analyzed to account for 96.92% of the total peak area in a GC-MS chromatogram. It was found that the compounds with ten carbon atoms showed the largest proportion. In the small-scale dry cleaning process (3 kg of laundry and 40 min of drying time), a total of 36 VOCs was quantified, and the odor contribution of these compounds was evaluated. The sum of the odor quotient (SOQ) was analyzed up to 151±163 in the first 12 min of operation. The main odor-causing compounds were acrolein, ethylbenzene, hexane, acetone, and decane, and their odor contributions were 32.28%, 13.47%, 10.52%, 10.20%, and 8.08%, respectively.