LAUSR

The advent of policies that incentivize or require alternative diesel fuels has increased the demand for the development of fast analytical methods aiming for the quality control of these fuels. This study approached an alternative method for the determination of biodiesel acidity employing capillary zone electrophoresis based on free fatty acids screening and quantification. Sample preparation comprised vortex‐assisted liquid‐liquid extraction of free fatty acids and was a crucial step for analysis. It was studied through a 32 full factorial design considering sample mass and the stirring time. Then, solvent suitability was evaluated univariately. The free fatty acid screening was carried out employing a capillary zone electrophoresis method able to separate C16:0, C18:0, C18:1 n‐9, C18:2 n‐6, and C18:3 n‐3, major fatty acids in a variety of vegetable oils used for biodiesel synthesis. In addition to the straightforward sample preparation protocol, the running time of the developed method was only 12 min. Moreover, ultraviolet absorption indirect detection of analytes was approached to avoid analytes derivatization, considering the lack of chromophore groups in saturated fatty acids. Statistical tests did not evidence any significant differences in the biodiesel acidity determination expressed in percentage of free fatty acids when comparing the proposed capillary zone electrophoresis method and the traditional potentiometric titration approach within the 95% confidence interval, which demonstrates the suitability of this alternative method for the biodiesel quality control in routine.