School of Chemistry, University of Southampton, SO17 1BJ, United Kingdom.
J Magn Reson. 2011 Oct;212(2):460-3. doi: 10.1016/j.jmr.2011.08.021. Epub 2011 Aug 17.
The accurate temperature measurement of solid samples under magic-angle spinning (MAS) is difficult in the cryogenic regime. It has been demonstrated by Thurber et al. (J. Magn. Reson., 196 (2009) 84-87) [10] that the temperature dependent spin-lattice relaxation time constant of (79)Br in KBr powder can be useful for measuring sample temperature under MAS over a wide temperature range (20-296 K). However the value of T(1) exceeds 3 min at temperatures below 20K, which is inconveniently long. In this communication, we show that the spin-lattice relaxation time constant of (127)I in CsI powder can be used to accurately measure sample temperature under MAS within a reasonable experimental time down to 10 K.
在低温条件下,对魔角旋转(MAS)下的固体样品进行精确温度测量是困难的。Thurber 等人已经证明(J. Magn. Reson.,196(2009)84-87)[10],在很宽的温度范围内(20-296 K),(79)Br 在 KBr 粉末中的温度相关自旋晶格弛豫时间常数可用于测量 MAS 下的样品温度。然而,在低于 20 K 的温度下,T(1)的值超过 3 分钟,这非常不方便。在本通讯中,我们表明,(127)I 在 CsI 粉末中的自旋晶格弛豫时间常数可用于在合理的实验时间内准确测量 MAS 下的样品温度,低至 10 K。