scholarly journals Effects of radial radio-frequency field inhomogeneity on MAS solid-state NMR experiments

2021 ◽  
Vol 2 (1) ◽  
pp. 523-543
Author(s):  
Kathrin Aebischer ◽  
Zdeněk Tošner ◽  
Matthias Ernst

Abstract. Radio-frequency field inhomogeneity is one of the most common imperfections in NMR experiments. They can lead to imperfect flip angles of applied radio-frequency (rf) pulses or to a mismatch of resonance conditions, resulting in artefacts or degraded performance of experiments. In solid-state NMR under magic angle spinning (MAS), the radial component becomes time-dependent because the rf irradiation amplitude and phase is modulated with integer multiples of the spinning frequency. We analyse the influence of such time-dependent MAS-modulated rf fields on the performance of some commonly used building blocks of solid-state NMR experiments. This analysis is based on analytical Floquet calculations and numerical simulations, taking into account the time dependence of the rf field. We find that, compared to the static part of the rf field inhomogeneity, such time-dependent modulations play a very minor role in the performance degradation of the investigated typical solid-state NMR experiments.

2021 ◽  
Author(s):  
Kathrin Aebischer ◽  
Zdeněk Tošner ◽  
Matthias Ernst

Abstract. Radio-frequency field inhomogeneity is one of the most common imperfections in NMR experiments. They can lead to imperfect flip angles of applied radio-frequency (rf) pulses or to a mismatch of resonance conditions resulting in artifacts or degraded performance of experiments. In solid-state NMR under magic-angle spinning, the radial component becomes time-dependent because the rf-irradiation amplitude and phase is modulated with integer multiples of the spinning frequency. We analyze the influence of such time-dependent MAS-modulated rf fields on the performance of some commonly used building blocks of solid-state NMR experiments. This analysis is based on analytical Floquet calculations as well as numerical simulations taking into account the time dependence of the rf field. We find that compared to the static part of the rf-field inhomogeneity, such time-dependent modulations play a very minor role in the performance degradation of the investigated typical solid-state NMR experiments.


2019 ◽  
Author(s):  
Dongyu Zhang ◽  
Boris Itin ◽  
Ann E. McDermott

AbstractSolid state NMR is a powerful tool to probe membrane protein structure and motions in native lipid structures. Sample heating, caused by magic angle spinning and radio frequency irradiation in solid state NMR, produces uncertainties in sample temperature and thermal broadening caused by temperature distributions, which can also lead to sample deterioration. To measure the sample temperature in real time, and to quantify thermal gradients and their dependence on radio frequency irradiation or spinning frequency, we use the chemical shift thermometer TmDOTP, a lanthanide complex. Compared to other NMR thermometers (e.g., the proton NMR signal of water), the proton spectrum of TmDOTP exhibits higher thermal sensitivity and resolution. In addition, the H6 proton in TmDOTP has a large chemical shift (−175 ppm at 275 K) and is well resolved from the rest of the proton spectrum. We identified two populations of TmDOTP, with differing temperatures and dependency on the radio frequency irradiation power, within proteoliposome samples. We interpret these populations as arising from the supernatant and the pellet, which is sedimented from the sample spinning. Our results indicate that TmDOTP is an excellent internal standard for monitoring temperatures of biophysically relevant samples without distorting their properties.


2016 ◽  
Vol 4 (34) ◽  
pp. 13183-13193 ◽  
Author(s):  
Ryohei Morita ◽  
Kazuma Gotoh ◽  
Mika Fukunishi ◽  
Kei Kubota ◽  
Shinichi Komaba ◽  
...  

We examined the state of sodium electrochemically inserted in HC prepared at 700–2000 °C using solid state Na magic angle spinning (MAS) NMR and multiple quantum (MQ) MAS NMR.


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