There is a substantial amount of literature dealing with many aspects of synthesis and characterization of pure and doped binary compounds including Mn-doped ZnO which has been widely studied due to its superb properties as a dilute magnetic semiconductor (DMS). Aspects concerning doping limits for these compounds is an important stage in the search for new materials. Samples of Zn1-xMnxO nanocrystal were synthesized at temperatures of 180 °C and 200 °C using wet or liquid phase synthesis method. Dopant concentrations x=0.5, 1, 1.5, 2, 2.5, 5, 10, 20, 30, 40 and 50 per cent were studied. Powder x-ray diffraction (PXRD) patterns of the samples were analyzed with a view to determining the onset of secondary phases and hence the solubility limit of the dopant. The solubility limit for Mn in ZnO samples synthesized at temperature of 200 °C is realized at x <20%. For samples synthesized at temperature of 180 °C, the solubility limit is x <0.5%.