With recent advances in magic angle spinning (MAS) technology, commercially available MAS probes can now achieve MAS rates exceeding 100 kHz. The very fast MAS system is characterized by tiny rotors with a diameter less than 1 mm, a sample volume less than 1 μL, and a strong rf-field strength close to 1 MHz. Due to these extreme features, careful handling of hardware and precise setup of experimental conditions is imperative for very fast MAS measurements. The primary objective of this chapter is to furnish a comprehensive and practical guide for establishing fundamental experimental conditions including both sample-independent and sample-dependent variables, related to very fast MAS techniques. Detailed discussions cover shimming, magic angle adjustment, rf-field strength calibration, frequency referencing, repetition delay, and fluctuations in spinning rate. In addition, the chapter introduces two widely used two-dimensional (2D) measurements: 1H homonuclear double-quantum/single quantum (DQ/SQ) correlations and X/1H cross-polarization heteronuclear single quantum coherence (CP-HSQC) experiments.

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Solid-State NMR Under Ultra-Fast MAS Rate of 40–120 kHz

  • Yusuke Nishiyama

摘要

With recent advances in magic angle spinning (MAS) technology, commercially available MAS probes can now achieve MAS rates exceeding 100 kHz. The very fast MAS system is characterized by tiny rotors with a diameter less than 1 mm, a sample volume less than 1 μL, and a strong rf-field strength close to 1 MHz. Due to these extreme features, careful handling of hardware and precise setup of experimental conditions is imperative for very fast MAS measurements. The primary objective of this chapter is to furnish a comprehensive and practical guide for establishing fundamental experimental conditions including both sample-independent and sample-dependent variables, related to very fast MAS techniques. Detailed discussions cover shimming, magic angle adjustment, rf-field strength calibration, frequency referencing, repetition delay, and fluctuations in spinning rate. In addition, the chapter introduces two widely used two-dimensional (2D) measurements: 1H homonuclear double-quantum/single quantum (DQ/SQ) correlations and X/1H cross-polarization heteronuclear single quantum coherence (CP-HSQC) experiments.