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In recent decades, thermochemical conversion of lignocellulosic biomass has gained popularity as a means to supplement or replace petroleum. Fast pyrolysis bio-oils have emerged as a potential source for transportation fuels and value-added chemicals. A lack of molecular-level understanding has stalled progress toward fast pyrolysis as an economically feasible option. To address this roadblock, this research focuses on high resolution mass spectrometry (HRMS) applications to molecular-level understanding of biomass pyrolysis. Negative mode atmospheric pressure photionization (APPI) and Fourier transform ion cyclotron resonance (FTICR) mass spectrometry (MS) are applied to nitrogen-rich switchgrass bio-oil and gasification tar for characterization and comparison. When compared with (+) APPI and positive and negative electrospray ionization, (-) APPI ionizes a wider range of compounds and provides a more comprehensive overview of the compounds present. The compounds accessed by (-) APPI are also generally accessed by one of the other ionization methods, but (-) APPI ionizes them with less specificity for a single group of compounds. A novel HRMS system for biomass pyrolysis analysis is introduced. Gas chromatography is coupled with dopant-assisted atmospheric pressure chemical ionization (dAPCI) for analysis by a time-of-flight mass spectrometer (TOF MS). Ammonia gas serves as the dopant. The ammonium adduct ions prevent the fragmentation observed in dopant-free APCI. Water plays a crucial role in the ionization

High resolution mass spectrometry to explore molecular-level understanding of biomass pyrolysis