The lithium concentration in an Al‐2.5 at% Li alloy is found to decrease after heating the alloy for different intervals at 560 °C then quenching it to room temperature. Dilatometric, electrical resistivity, and internal friction measurements are used to study the Li loss from the alloy which is found to start above 245 °C. The total amount of Li loss is found to depend linearly on temperature. The analysis of the results proves that the process of the Li loss is controlled primarily by a surface reaction.