The temperature dependence of the 23NaOH pure quadrupole resonance (NQR) frequency has been studied from 77 to 550 K and shows a change in slope and a discontinuous change in frequency of 6 ± 2 kHz at the orthorhombic to monoclinic phase transition at 505 K. At 292 K the 23Na NQR frequency is 1.778 ± 0.001 MHz, 11 <0.04. The temperature dependence ofthe deuterium quadrupole coupling was fit to a librating molecule model between 293 and 570 K (QCC = 245 ± 2 kHz, 11 = 0.05 ± 0.01 at 293 K) and confirms that the frequency ofthe ODlibration decreases in the high temperature monoclinic phase.