Coal-fired power plants emit various Particulate Matter(PM) at coal storage pile and ash landfill as well as the stack, and affect the surrounding environment. Field Emission Scanning Electron Microscopy and Energy Dispersive X-ray analyzer(FE-SEM/EDX) were used to develop identification factor and the physico-chemical analysis of PM emitted from a power plant. In this study, three samples of pulverized coal, bottom ash, and fly ash were analyzed. The pulverized coal was spherical particles in shape and the chemical composition of C-O-Si-Al and C/Si and C/Al ratios were 200~300 on average. The bottom ash was spherical or non-spherical particles in shape, chemical composition was O-C-Si-Al-Fe-Ca and C/Si and C/Al ratios were 4.3±4.6 and 8.8±10.0. The fly ash was spherical particles in shape, chemical composition was O-Si-Ai-C-Fe-Ca and C/Si and C/Al ratios were 0.5±0.2 and 0.8±0.5.