Methodological and experimental aspects of the estimation of transient heat transfer coefficients in quenching experiments, using inverse heat transfer methods, were addressed and investigated. Beck’s method was used for the estimation of the transient heat transfer coefficient history from interior transient temperature measurements during quenching. Experiments involved plunging a high-purity copper sphere into cooling baths without boiling. The sphere was instrumented with several interior thermocouples for measuring the transient temperature response during quenching. Water and ethylene glycol were investigated. The early transient values of the heat transfer coefficient history were found to be about 100–120 percent higher than the values predicted using well-known empirical correlations for free convection. The later time values were in good agreement with those predicted with empirical correlations. The transient inverse technique has the capability of estimating early transients and subsequent quasi-steady-state values of heat transfer coefficient in a single transient experiment.