Abstract: Gases evolved during photolithographic processing of chemically amplified photoresist systems are monitored to allow optimization of process parameters such as intensity and duration of applied heat or radiation. Specifically, during soft bake, evaporation of solvent gases is detected. During exposure and PEB, gases evolved during activation of the polymer resin component by the photoacid are detected. The intensity and/or duration of the heating or exposure are then varied to optimize resolution of the particular photolithography process. Residual gas analysis, diode laser spectroscopy, FT-IR spectroscopy, and electronic sensing may be utilized alone or in combination to monitor composition and/or concentration of evolved gases in accordance with the present invention.