Crystalline, pure or Mn-doped ZnGa2O4 powders have been prepared in situ in urea (with or without enzyme urease)-containing Zn and Ga nitrate (and Mn nitrate) solutions by simply holding those for 24–48 h, at 90 °C, in screw-capped glass bottles in a constant-temperature laboratory oven. Single-phase pure or Mn-doped zinc gallate powders synthesized with the spinel crystal structure had an average particle size around 15 to 18 nm. Powders were characterized by x-ray diffraction, scanning electron microscopy, energy-dispersive x-ray spectroscopy, inductively-coupled plasma atomic emission spectroscopy, simultaneous thermogravimetry and differential thermal analysis, Fourier-transformed infrared spectroscopy, and carbon and nitrogen analyses. Calcination behavior of the as-filtered powders was later studied in an air atmosphere over the temperature range of 90 to 1200 °C.