Kitamura Masashi, Asano Atsushi
Department of Applied Chemistry, National Defense Academy.
Anal Sci. 2013;29(11):1089-93. doi: 10.2116/analsci.29.1089.
We investigated temperature distribution in a solid state nuclear magnetic resonance (NMR) sample rotor under magic angle spinning (MAS) experiments by analyzing the (207)Pb chemical shift of solid lead nitrate (Pb(NO3)2). The analysis corrected a mismatch of the temperature dependence of (1)H spin-lattice relaxation time (T1(H)) obtained from different sample positions in the rotor. We prepared three rotors that consisted of Pb(NO3)2 partitioned into the three different parts with Teflon spacers, and measured the temperature distribution related to the placement using the prepared three rotors. The obtained temperature distribution showed a large gradient in the sample rotor. The temperature distribution was related to the placement in the rotor and successfully visualized. Finally, the divergent temperature dependence of T1(H) obtained at different placement positions in the sample rotor was successfully corrected to accurate temperature dependence.
我们通过分析固体硝酸铅(Pb(NO₃)₂)的²⁰⁷Pb化学位移,研究了在魔角旋转(MAS)实验下固态核磁共振(NMR)样品转子中的温度分布。该分析校正了从转子中不同样品位置获得的¹H自旋 - 晶格弛豫时间(T₁(H))的温度依赖性不匹配问题。我们制备了三个转子,其中Pb(NO₃)₂被聚四氟乙烯垫片分隔成三个不同部分,并使用制备的三个转子测量了与放置位置相关的温度分布。所获得的温度分布显示样品转子中存在较大梯度。温度分布与在转子中的放置位置有关,并成功实现了可视化。最后,成功校正了在样品转子不同放置位置获得的T₁(H)的发散温度依赖性,使其具有准确的温度依赖性。