Precipitation behavior of metastable phases in an Al-1.94 at%Cu alloy during isothermal aging at 373 K was investigated by means of Vickers microhardness tests, DSC measurements and TEM observations. The size distribution of the precipitates was quantitatively investigated based on the TEM, HRTEM and HAADF-STEM images, and statistical parameters that fit the precipitate size distribution were determined under a log-normal distribution approximation. We have successfully estimated the volume fraction of copper in precipitates, and found that the G.P.(II) formation results in increases of volume fraction of metastable particles, mean size and hardness.