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Fractional distillation of industrial wood pyrolitic tar in the temperature range 125–265 °C was performed and highest heat of combustion for each fraction was determined by combustion bomb calorimetry. It was demonstrated that multidimentional analysis method could reveal a good correlation with r = 0,99 between calorific value and Near-IR-spectra characteristics which were recorded for each fraction. Application of this method to a large-scale production of wood pyrolytic biofuels could serve as a new analytic method for fuel calorific value determination.