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Globally, there are vast amounts of low-grade heat sources from industrial waste and renewables that can be converted into electricity through advanced thermodynamic power cycles and appropriate working fluids. In this thesis, experimental research was conducted to investigate the performance of a small-scale Organic Rankine Cycle (ORC) system under different operating conditions. The experimental setup consisted of typical ORC system components, such as a turboexpander with a high speed generator, a scroll expander, a finned-tube condenser, an ORC pump, a plate evaporator and a shell and tube evaporator. R245fa was selected as the working fluid, on account of its appropriate thermophysical properties for the ORC system and its low ozone depletion potential (ODP). The test rig was fully instrumented and extensive experiments carried out to examine the influences of several important parameters, including heat source temperature, ORC pump speed, heat sink flow velocity, different evaporators and with or without a recuperator on overall R245fa ORC performances. In addition, in terms of the working fluid’s environmental impact, temperature match of the cycle heat processes and system compactness, CO2 transcritical power cycles (T-CO2) were deemed more applicable for converting low-grade heat to power. However, the system thermal efficiency of T-CO2 requires further improvement. Subsequently, a test rig of a small-scale power generation system with T-CO2 power cycles was developed with essential components connected; these included a plate CO2 supercritical heater, a CO2 transcritical turbine, a plate recuperator, an air-cooled finned-tube CO2 condenser and a CO2 liquid pump. Various preliminary test results from the system measurements are demonstrated in this thesis. At the end, a theoretical study was conducted to investigate and compare the performance of T-CO2 and R245fa ORCs using low-grade thermal energy to produce useful shaft or electrical power. The thermodynamic models of both cycles were developed and applied to calculate and compare the cycle thermal and exergy efficiencies at different operating conditions and control strategies. In this thesis, the main results showed that the thermal efficiency of the tested ORC system could be improved with an increased heat source temperature in the system with or without recuperator. When the heat source temperature increased from 145 oC to 155 oC for the system without recuperator, the percentage increase rates of turbine power output and system thermal efficiency were 13.6% and 14% respectively while when the temperature increased from 154 oC to 166 oC for the system with recuperator, the percentage increase rates were 31.2% and 61.97% respectively. In addition, the ORC with recuperator required a relative higher heat source temperature, which is comparable to a system without recuperator. On the other hand, at constant heat source temperatures, the working fluid pump speed could be optimised to maximise system thermal efficiency for ORC both with and without recuperator. The pressure ratio is a key factor impacting the efficiencies and power generation of the turbine and scroll expander. Maximum electrical power outputs of 1556.24W and 750W of the scroll expander and turbine were observed at pressure ratio points of 3.3 and 2.57 respectively. For the T-CO2 system, the main results showing that the CO2 mass flow rate could be directly controlled by varying the CO2 liquid pump speeds. The CO2 pressures at the turbine inlet and outlet and turbine power generation all increased with higher CO2 mass flow rates. When CO2 mass flow rate increased from 0.2 kg/s to 0.26kg/s, the maximum percentage increase rates of measured turbine power generation was 116.9%. However, the heat source flow rate was found to have almost negligible impact on system performance. When the thermal oil flow rate increased from 0.364kg/s to 0.463kg/s, the maximum percentage increase rate of measured turbine power generation was only 14.8%. For the thermodynamic analysis, with the same operating conditions and heat transfer assumptions, the thermal and exergy efficiencies of R245fa ORCs are both slightly higher than those of T-CO2. However, the efficiencies of both cycles can be enhanced by installing a recuperator at under specific operating conditions. The experiment and simulation results can thus inform further design and operation optimisations of both the systems and their components.