Nanosized EMT-type zeolite crystals in sodium (Na-EMT) and ion-exchanged lithium (Li-EMT) forms were prepared. The sorption behavior of Li(Na)-EMT samples towards water, methanol and a mixture of both (50:50) was studied by combined thermogravimetric and infrared spectroscopic methods. The stability of the samples prior to and after the sorption measurements in two subsequent cycles was confirmed by X-ray diffraction, N2 sorption and NMR spectroscopy. The high sorption capacity of the Li-EMT sample towards water was demonstrated. It was found that the methanol is replaced by water faster in the Li-EMT sample in comparison to the Na-EMT sample. At low temperature, the methanol shows weak adsorption on each cationic site and no side products during desorption for both samples were obtained.