Thick electrodeposits of 24K gold were prepared from 14 types of plating solutions in both new and replenished‐used conditions. The deposits were examined by x‐ray, scanning electron microscope, gravimetric, and electrical techniques. It was found that the purity, microstructure, and apparent density were functions of the plating solution type and age. The crystal lattice constants were found to be independent of both type and age.