Department of Physics, University of Warwick, Coventry CV4 7AL, UK.
J Magn Reson. 2010 May;204(1):169-72. doi: 10.1016/j.jmr.2010.02.018. Epub 2010 Feb 21.
The measurement of temperature in a Magic Angle Spinning NMR probe in the temperature range 85-300K is discussed. It is shown that the shift of the (119)Sn resonance of Sm(2)Sn(2)O(7) makes a good thermometer with shift being given by delta=223 - 9.54x10(4)/Tppm and a potential precision of better than 0.5K over the entire temperature range. The sensitivity is such (e.g. 4.2ppm/K at 150K) that small temperature gradients across the sample can readily be measured. Furthermore, since the spin-lattice relaxation time is very short, measurements can be made in approximately 1s enabling relatively rapid temperature changes to be followed. Values for the chemical shift of (207)Pb in Pb(NO(3))(2) down to approximately 85K are also presented. Although the (207)Pb shift variation is approximately linear near room temperature (we find a slope 0.725+/-0.002ppm/K over the range 293-153K), it clearly deviates from linearity below approximately 130K.
讨论了在 85-300K 温度范围内 Magic Angle Spinning NMR 探头中温度的测量。结果表明,Sm2Sn2O7 中(119)Sn 共振的位移是一种很好的温度计,其位移由 delta=223 - 9.54x10(4)/Tppm 给出,在整个温度范围内的精度优于 0.5K。灵敏度非常高(例如在 150K 时为 4.2ppm/K),因此可以很容易地测量样品中微小的温度梯度。此外,由于自旋晶格弛豫时间非常短,因此可以在大约 1s 内进行测量,从而可以跟踪相对快速的温度变化。还给出了 Pb(NO3)2 中(207)Pb 的化学位移值,低至约 85K。尽管(207)Pb 位移的变化在室温附近大致呈线性(我们发现在 293-153K 的范围内斜率为 0.725+/-0.002ppm/K),但在约 130K 以下明显偏离线性。