The basic zirconium sulfate was prepared from ZrOCl2.8H2O and H2SO4 in the 9$0^{circ}C$ aqueous solution. The pH and amount of unreacted zirconium in the solution that reacton had completed was 0.2 and 10%. As the pH was increased to 1.4 by NH4OH theresulting precipitates were the mixtures of the basic zirconium sulfate and the zirconium hydroxide although the precipitates were recovered completely. The thermal decomposition behavior of this sample has been examined by thermal analysis(TG-DTA), X-ray diffraction study, infrared spectroscopy and sulfur analysis. As a result, it was found that the precipitates have perfectly been decomposed at 85$0^{circ}C$ accompanying to the release of a molecule of water below 25$0^{circ}C$ and 85% sulfate at about $600^{circ}C$. The thermally decomlposed products were initially amorphous phase, which were become metastable tetragonal phase with increment of temperature and finally transformed to the stable monoclinic phase at 100$0^{circ}C$.