Investigations of the Rankine cycle for power generation using waste heat from a cement plant were performed, while considering three waste streams of three different temperature ranges. Six organic fluids, in addition to water, were selected to be employed as working fluids in five suggested Rankine cycle schemes built and simulated with Aspen HYSYS v8.8. The suggested schemes were made to suit the types of the working fluids used in the investigations. Working fluids were compared based on efficiency to select the best organic fluid to be compared with water. The basic comparisons resulted in the selection of seven methanol points in scheme 5 (based on the turbine inlet pressures) to be compared with nine points of water in schemes 1 and 4. The comparisons showed that methanol resulted in the highest net power output and cycle efficiency with the lowest irreversibility. Furthermore, the selected methanol points showed the highest net power output values, in addition to the lowest payback period of 4 years with high net present values. Consequently, methanol is suggested as a better choice for working fluid in Rankine cycle for waste heat recovery in the cement industry.