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Ultrasound has been widely used as a technological alternative way to analyse noninvasively an assortment of materials. It includes liquids with dissimilar physical characteristics, including mono-and multi-phasic mixtures, suspension formation and dissolution, in-line processing, among other practical applications. Regardless the huge spread of uses, so far ultrasound has not been proved to be able to quantify transesterification kinetics with a metrological approach. The aim of this chapter is to demonstrate that a properly designed ultrasonic experiment can be developed to identify remarkable stages of a transesterification reaction to produce biodiesel. The method was compared both with gas chromatography and hydrogen nuclear magnetic resonance ( 1 H NMR). For an in-line application, ultrasound has been proved to work properly as a monitoring tool for chemical reaction kinetics.