The contents and proportions of hematite (α-Fe₂O₃) and goethite (α-FeOOH) in soil have a clear indication for climate, so it is an important scientific issue in paleoclimate research to semi-quantitatively and quantitatively identifying their contents. Heating experiments were conducted on loess-paleosol and red soil samples, the composition and diversities of goethite and hematite were analyzed by comparing the parameters of Diffuse reflectance spectrum; (DRS) peak value, red light section and chroma indexes (a*, b*, b*/a*), and meanwhile semi-quantitative reconstruction of goethite and hematite were discussed. The results showed that the first derivative configuration of DRS in loess samples were different from those of red soil samples. Goethite sub-peak was obvious in loess samples while hematite characteristic peak was distinct in red soil samples. Generally, the values of a* in red soil samples were higher than those of loess samples, and the diversity of b* between loess and red soil samples was not obvious. Moreover, the changes of a* and b* were synchronous in soil. The value of hematite characteristic peak in red soil or loess samples was significantly correlated to a*. The characteristic peaks of goethite were decreased and clay mineral peaks were shown in heating process, meanwhile the characteristic peaks of hematite were increased, which indicate that goethite dehydrates and transforms to hematite. During the heating process with aerobic participation, fine grain magnetite (Fe₃O₄) and unstable maghemite (γ-Fe₂O₃) may be the important contributors to hematite formation except the conversion of goethite into hematite.