Iron oxide is one of important minerals in modern soils and red paleosols, while the quantity and morphology of iron oxides are the critical indicators for soil-formation and weathering development. However, identification of iron oxides in soils and sediments is challenged by its small size, poor crystallinity, low content, close bond with clay minerals and the effect of soil matrix. Here the diffuse reflectance spectroscopy (DRS) method was adopted to quantify and semi-quantify iron oxides of red paleosols in Yuanmou Basin, southwest China. The spectral reflectance of paleosols was about 45%, measured over the range of 400～2 500 nm at an interval of 2 nm with a total of 1 061 bands. Nearly all samples exhibited the similar spectral reflectance, while the first and secondary derivative curve peaks occurred at 575 nm for hematite and 435 nm for goethite, respectively. Combination of CBD method and DRS technique the concentrations of hematite and goethitethe in red paleosols in Yuanmou Basin were 3~5 and 5~10 g·kg-1, respectively. The estimate on goethite and hematite using DRS was supported by the X-ray diffraction method.