Pneumatic angle adjustment for magic angle spinning spherical rotors
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Date
2021-06
Publication Type
Journal Article
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yes
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Abstract
Precise alignment of the sample’s spinning axis is vital for many magic angle spinning solid state NMR experiments. Spherical rotors are a new paradigm for magic angle spinning NMR, having been demonstrated to spin stably with little risk of rotor crash, but like cylindrical rotors, they have previously only utilized a mechanical adjustment method to set the sample’s rotation axis to the magic angle. Here we show that by using a second gas aperture within the stator, a spherical rotor’s axis of rotation may be precisely pitched about the magic angle without mechanical adjustment or motion of the stator. The 2H MAS sideband lineshape of the carboxylic acid deuteron resonance in d4-malonic acid is used as a measure of the rotor’s absolute deviation above or below the magic angle by comparing the experimental data to simulated lineshapes. We observe a linear, monotonic relationship between the angle adjustment gas flow rate and the rotor’s pitch angle, which is also accompanied by an increase in spinning rate. Precise and in operando control of the spinning axis angle is expected to have considerable advantages to future implementation of MAS within narrow-bore magnets, and for variable angle spinning (VAS) and dynamic angle spinning (DAS) experiments.
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Publication status
published
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Book title
Journal / series
Volume
6–7
Pages / Article No.
100014
Publisher
Elsevier
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Edition / version
Methods
Software
Geographic location
Date collected
Date created
Subject
Angle adjustment; Spherical rotor; MAS; Pneumatic; NMR hardware; Solid state NMR
Organisational unit
09681 - Barnes, Alexander / Barnes, Alexander