A variety of degradation products are produced upon pretreatment of lignocellulosic biomass with dilute acid. To date, the complexity of these samples has significantly limited the scope of efforts to perform summative analyses of degradation products. Qualitative and quantitative interrogation of hydrolysates is also paramount to identifying potential correlations between pretreatment chemistry and microbial inhibition in downstream bioconversion processes.

Chromatographic techniques have been used in combination with mass spectrometry (i.e., HPLC-MS/MS and GC/MS) to qualitatively identify dozens of organic degradation products (e.g., organic acids, phenols, aldehydes, etc.) in corn stover pretreatment hydrolysates. Additionally, a developing suite of analytical methodologies based on chromatographic separation of analytes with ultraviolet, MS, and/or flame ionization detection modes has been applied to perform quantitative assessments of a variety of hydrolysate components as a function of pretreatment time, temperature, and pH. Correlations of product concentrations to the pretreatment severity function indicate differing responses of various compounds to the kinetic influences of temperature and reaction time.