Freezing points for aqueous monoethanolamine (MEA), methyl diethanolamine (MDEA), and MEA−MDEA solutions were measured in the concentration range from 0 to 0.4 mass fractions of the alkanolamines. For the aqueous MEA−MDEA system, freezing points for 1:4, 1:2, 1:1, 2:1, and 4:1 molar ratios of MEA/MDEA were determined. The experimental values indicate that the MDEA−water interaction is stronger than the MEA−water interaction. Measurements were carried out by a new modified Beckmann apparatus, which has not previously been described. The apparatus and method proved to have good repeatability and accuracy. A correlation of the freezing points as functions of the solution composition was made. Measurements of aqueous MEA and aqueous MDEA were compared to experiments found in the open literature.