The determination of the chemical composition of lignocellulosic material is a resource-consuming analytical challenge that usually requires several chromatography-based techniques. Minor cell wall components and degradation products are, therefore, often ignored. 1H NMR spectroscopy applied to acid hydrolysates offers a quicker and more complete means to analyze lignocellulosic materials. Excellent agreement with standard techniques was observed for d-glucose, d-mannose, d-xylose, l-arabinose, acetic acid, furfural and 5-hydroxymethyl furfural in the three examined lignocellulosic materials. Determination of d-galactose and cellobiose in the hydrolysates resulted in higher values when determined by 1H NMR spectroscopy compared to chromatography. d-Galacturonic acid, formic acid and levulinic acid could also be quantified by 1H NMR spectroscopy. Consequently higher yields (more complete mass closures) were achieved giving a more comprehensive picture of the chemical composition of the original lignocellulosic material. The 1H NMR technique appears to be advantageous especially when sugar degradation products are of interest, e.g. when studying the potential of lignocellulosics as biofuel precursors.