1. Purpose

There are many NMR experiments that are performed at different temperatures or where the emphasis lies on the measurement of a temperature-dependent effect. Hence, it is most important to know whether the temperature controller of the instrument used gives a correct reading of the actual temperature within the sample. Many different calibration samples have been proposed, working at different temperature ranges and for different nuclides. Here we restrict the description to the most common low temperature standard, methanol, where the chemical shift difference between the OH proton and those of the methyl group is used for the calibration. The literature [3–8] proposes different techniques and standards for different nuclides in the solid and liquid states.

2. Literature

A. L. van Geet, Anal. Chem. 1970, 42, 679–680; ibid. 1968, 40, 2227–2229.
A. G. Webb, Ann. Rep. NMR Spectrosc. 2002, 45, 1–67.
H. Friebolin, G. Schilling, L. Pohl, Org. Magn. Reson. 1979, 12, 569–573.
C. Piccinni-Leopardi, O. Fabre, J. Reisse, Org. Magn. Reson. 1976, 8, 233–236.
F. H. Köhler, X. Xie, Magn. Reson. Chem. 1997, 35, 487–492.
H. Quast, M. Heubes, A. Dunger, H.H. Limbach, J. Magn. Reson. 1998, 134, 236–244.
W. H. Sikorski, A. W. Saunders, H. J. Reich, Magn. Reson. Chem. 1998 36, S118–S124.
N. M. Loening, J. Keeler, J. Magn. Reson. 2002, 159, 55–61.

3. Pulse Scheme and Phase Cycle

Single-pulse proton sequence for methanol temperature calibration