A rapid method is needed to assess biogas and methane yield potential of various kinds of substrate prior to anaerobic digestion. This study reports near infrared reflectance spectroscopy (NIRS) as a rapid alternative method to the conventional batch methods for prediction of specific biogas yield (SBY), specific methane yield (SMY) and kinetics of biogas yield (k-SBY) of reed canary grass (RCG) biomass. Dried and powdered RCG biomass with different level of maturity was used for biochemical composition analysis, batch assays and NIRS analysis. Calibration models were developed using partial least square (PLS) regression from NIRS spectra. The calibration models for SBY (R2 = 0.68, RPD = 1.83) and k-SBY (R2 = 0.71, RPD = 1.75) were better than the model for SMY (R2 = 0.53, RPD = 1.49). Although the PLS model for SMY was less successful, the model performance was better compared to the models based on chemical composition.