Fast quantification of water content in glycols by compact ¹H NMR spectroscopy

Glycols are key chemicals for many applications in different fields of activities. Being highly hydroscopic, glycols contain usually water. The presence of water, even in tiny amounts, can affect their chemical and physical properties. Therefore, the accurate determination of water content is essential for any intended applications. In this context, a novel method using low-field Nuclear Magnetic Resonance (NMR) spectroscopy is introduced. The proposed approach offers a straightforward, fast, low-cost, and versatile solution for water quantification in glycols without the need for reagents or calibration data. It is demonstrated by quantifying the water concentration up to 11 wt% in aqueous ethylene glycol (EG) and triethylene glycol (TEG) mixtures with the help of lineshape analysis of the corresponding proton spectra. The limit of detection, achieved within 1 min of measuring time, was 0.05 wt% for water in EG and 0.15 wt% in TEG. The excellent agreement between the NMR results and those from the Karl-Fischer titration indicates that the proposed NMR-based approach has a great potential to be used as an alternative to the Karl-Fischer method. In addition, it is expected that the same methodology can be applied for water quantification in more complex glycolic solutions and other mixtures.