Rapid or on-line coal analysis is of great interest in coal industry as it would allow efficient plant operation. Multivariate analysis has been applied to near-infrared(NIR) spectra coal for investigating the relationship between coal properties(%) (moisture, ash, volatile matter, fixed carbon, carbon, hydrogen, nitrogen, oxygen, sulfur), heating value(kcal/kg) and corresponding near-infrared spectral data. The quantitative analysis was carried out by applying PLS(partial least squares regression) to determine a methodology able to establish a relationship between coal properties and NIR spectral data being applied mathematical pre-treatments for minimizing the physical features of the samples. As a results of the analysis, this technique is able to classify the species of coals and to predict the all coal properties except ash, nitrogen and sulfur. The efficient operation of coal fired power plant is expected owing to real time on-line coal analysis of moisture and heating value.