Biodiesel is an important building block in renewable energy transformation. The main issue is that during storage biodiesel will undergo transformation processes that can lead to molecular changes, which then can cause applicational problems such as severe motor damage. To prevent this, a detailed understanding of the involved molecules and the emerging aging products is necessary. Biodiesel samples were stored for up to 12 months to monitor molecular changes, and all mixtures were investigated by using ultrahigh-resolution mass spectrometry (HRMS) with electrospray ionization (ESI). The data revealed that during storage large numbers of oxygen atoms were incorporated into the fatty acid methyl esters (FAMEs). This process was dominant for the first quarter of aging but then became overshadowed by dimerization of oxygenated FAMEs. This means that there are two main pathways for aging in biodiesel: polyoxygenation and oligomerization. These findings greatly pin down the possible causes for sedimentation giving a solid foundation for aging inhibition development.

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Due to a trend to higher sustainability, biodiesel is often mixed into petrodiesel. The analysis of these blends on a molecular level is not trivial, since huge differences in concentrations and polarity of the analytes require a large dynamic range of the analytical method, as well as the ability to investigate molecules of widely different polarities. A combination of high-performance liquid chromatography (HPLC) with high resolution mass spectrometry (HRMS) was identified as a promising method and a normal-phase (NP)-HPLC using amino-functionalized silica gel-based stationary phase delivered the best results with very fast (under 4 min) measurements, with distinct separation of the compounds and clean mass spectra of singular compounds. This method can also be easily modified to elute all FAMEs (fatty acid methyl esters) in one singular peak, thus making the separation even faster (under 3 min).

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