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Qualitative and quantitative assessment of total sulfur and sulfur species in solid phase is necessarily important for development of effective desulfurization methods, reduction of environmental pollution, and prevention of catalyst poisoned. In this work, TPO-IR (Temperature Programmed Oxidation- Infrared) method was used for rapid determination of sulfur species in solid minerals. The high purity of Ag2S was used as the calibration materials at the fixed temperature of 1100 °C, and the TPO experimental runs were performed on the solid minerals of phosphorite and coal. The results show that pyrite sulfur with Tmax of 426 °C, and two thiophene sulfurs with Tmax of 450 °C and 481 °C were found in Kaiyang phosphorite by fitting the TPO-IR curves; while pyrite sulfur with Tmax of 432 °C, complex sulfide with Tmax of 679 °C and sulfate sulfur with Tmax of 939 °C were found in Weng’an phosphorite. For Gas coal, the TPO-IR curves of sulfur release can be deconvoluted into seven individual curves, while that of Anthracite deconvoluted into four individual curves. In conclusion, the TPO-IR method has many advantages for determination of sulfur species in solid phase systems, such as less sample consumption, simple pretreatment, convenient operation and low cost, etc.