Boiling heat transfer is extensively used in various industrial applications to efficiently dissipate a large amount of heat by maintaining lower surface temperatures. The maximum heat flux dissipated during boiling is limited by the critical heat flux (CHF) and limited visualization of the boiling surface limits the identification of the impending CHF condition to rely on temperature monitoring alone. The study presented here focuses on developing a method for analyzing and identifying acoustic signatures throughout the nucleate boiling regimes that are indicative of the boiling state of the heater surface. The bubble nucleation and coalescence along with bubble collapse at the liquid-vapor interface leads to variation in acoustic emission patterns during boiling. These sound waves are studied and acoustic signatures that are representative of the impending CHF are identified over plain and enhanced copper substrates with water as the working fluid. During pool boiling study, it was observed that sound was dominant in two frequency regions (400–500 Hz dominant throughout nucleate boiling and 100–200 Hz dominant at heat fluxes > 100 W/cm2). However, just before CHF, a sudden drop in amplitude was observed in the high frequency region (400–500 Hz), while the amplitude in low frequency region (100–200 Hz) continued to rise. It was concluded that this acoustic study can be used as a tool to predict the approaching CHF condition.