The CO2-, CH4-, and CO2/CH4-loaded β-form hydroquinone (HQ) clathrates were synthesized by the gas phase reaction between α-form HQ and high pressure gases. Temperature-dependent Raman spectra of guest-free, CO2-loaded, CH4-loaded, and CO2/CH4-loaded β-form HQ clathrates were measured in the temperature range 300−385K at increments of 5 K. The CH4 molecules rapidly escaped from the β-form HQ clathrate in the temperature range 360−380 K, whereas the CO2 molecules were gradually released from the β-form HQ clathrate framework in the wide temperature range 300−380 K. It was also found that both CO2 and CH4 molecules were rapidly released from the CO2/ CH4-loaded β-form HQ clathrate framework in the temperature range 360−380 K. However, all of the guest-free and guest-loaded β-form HQ clathrates were fully converted to the α-form HQ at the same temperature of 385 K. These results demonstrate the strong effect of temperature on both guest−host interactions and the stability of the framework structure.