Scanning electron microscopy, X-ray diffractometry, Xray absorption spectroscopy, and other means are used to investigate the effect of thermal treatment temperature, 105-1100°C, on the immobilization of nickel (Ni) by the inorganic oxides of latosol. Ni is more firmly immobilized by the latosol with increasing temperature. Spectral analyses indicate that a shoulder toward the edge-jump appears in the spectra of X-ray absorption near-edge structure for the samples heated at 900 and 1100°C. Moreover, the intensity of the main peak at the edge increases with higher temperature; this information indicates the distortion of the divalent nickel [Ni(II)] environment in the samples heated at 900 and 1100°C. Nevertheless, the distortion is absent from the samples heated at 105 and 500°C. The fact of the distortion of the Ni(II) environment suggests the occurrence of a chemical reaction between the Ni compound and the inorganic matrices of the latosol soil during the heating process at 900 and 1100°C. In addition, the extended X-ray absorption fine structure results correspond well to the X-ray absorption near-edge structure results; the former are supportive of the occurrence of a distorted Ni(II) environment in the samples heated at 900 and 1100°C. The wet-chemistry results show that the samples heated at 900 -1100°C leach less Ni than the 105-500°C samples do. The change of the Ni environment is related to the observation that less Ni is leached from the samples heated at 900 -1100°C. Furthermore, the pore closing phenomenon is observed only in the 1100°C sample; this phenomenon corresponds with the fact that the 1100°C sample leaches less Ni than the 900°C sample does.