FTIR spectroscopy together with multicomponent partial least-squares (PLS) method was used for the determination of moisture content, ash and volatile combustible in coal. For forty-eight coal samples from five mines in the Ostrava-Karviná region, the parameters were first determined by standard procedures. IR spectra of coal samples measured in KBr tablets and by diffuse reflectance were used for construction of calibration models by the PLS method. The classical and PLS methods gave the same results. Uncertainties in the above determinations were found by repeated measurements of IR spectra using the PLS method.