In order to investigate benchtop NMR spectroscopy as a monitoring tool for fermentation processes, we used a barley malt mash and took various samples over time and analysed them by NMR spectroscopy with 3-(trimethylsilyl)-2,2,3,3-tetradeuteropropionic acid sodium salt (TSP-d4) as an internal standard for the quantification of ethanol and validated the results by two different enzymatic standard test kits for ethanol analysis. We could show that the results between NMR spectroscopy and test kits were consistent with NMR having a much lower standard deviation. Finally, we discussed the applicability of the method as well as the possibility to quantify various other substances.