The red, tetragonal form of lead oxide, α-PbO, litharge, has been synthesized in the nanoparticle range using a rapid, one-step reaction sequence using water as the reaction medium. The product was characterized by powder x-ray diffraction and scanning electron microscopy. With time at room temperature, the original material slowly changed in color intensity, indicating its alteration to β-PbO, massicot. Grinding the aged material converted it back to the original litharge form. The role of impurities in the experimental synthesis of the material and microstructural variations in the final product are discussed, along with the PbO-phase compositions of commercial products.