For the first time, we report on the application of a tapered element oscillating microbalance (TEOM) as a novel technique to investigate the thermal decomposition of hydrotalcite-like compounds (HTlcs) in air. Experiments were performed in the temperature range of 323-973 K with Mg-Al, Ni-Al, and Co-Al-HTlcs. The TEOM technique measures mass changes based on inertial forces, presenting important advantages over conventional thermogravimetric analyzers, such as the very rapid time response and the well-defined flow pattern. In general terms, excellent agreement between TEOM, TGA, and DTA techniques during HTlc decomposition was obtained. Interestingly, transition temperatures in the TEOM were lower than in TGA and DTA, particularly for removal of interlayer water but also for dehydroxylation of the brucite-like layers and decarbonation. This was attributed to the flow-through operation in the tapered element of the TEOM as compared to the recognized gas stagnancy and bypass in sample crucibles of conventional thermogravimetric analyzers. Our results conclude that the TEOM technique is suitable for temperature-programmed studies. However, due to its operation principle, blank runs are required in contrast to the more automatic operation in commercial thermogravimetric units. Besides, a careful sample loading and packing in the micro-reactor is essential for reproducible results.