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NMR Spectrometers: Resolution and Error Correction01:14

NMR Spectrometers: Resolution and Error Correction

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When magnetic nuclei in a sample achieve resonance and undergo relaxation, the signal detected in NMR is an approximately exponential free induction decay. Fourier transform of an exponential decay yields a Lorentzian peak in the frequency domain. Lorentzian peaks in an NMR spectrum are defined by their amplitude, full width at half maximum, and position, where the peak width is governed by the spin-spin relaxation time alone. In real experiments, however, the applied magnetic field is rendered...
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NMR Spectrometers: Overview01:20

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NMR spectrometers consist of a strong magnet, a radiofrequency transmitter, and a detector attached to a computer console for recording spectra of samples containing NMR-active nuclei. In first-generation NMR instruments called continuous-wave spectrometers, the resonance frequencies of the nuclei are determined by frequency-sweep or field-sweep methods. The magnetic field strength is fixed and the rf signal is swept in the former, while the radiofrequency signal is fixed and the magnetic field...
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2D NMR: Overview of Homonuclear Correlation Techniques01:16

2D NMR: Overview of Homonuclear Correlation Techniques

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Homonuclear correlation spectroscopy (COSY) is a powerful technique used in Nuclear Magnetic Resonance (NMR) spectroscopy to study the correlations between nuclei of the same type within a molecule. It provides information about scalar couplings between adjacent nuclei, which helps determine connectivity and structural information. There are several COSY variants, each with its unique strengths and experimental parameters.
COSY90 is the standard two-dimensional (2D) COSY experiment that...
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Two-Dimensional (2D) NMR: Overview01:12

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The 1D NMR spectrum of large and complex molecules like natural products has complicated splitting patterns and overlapping signals, which can be easily interpreted using 2-dimensional (2D) NMR. Unlike 1D NMR, 2D NMR has two frequency axes that provide the coupling information between the nucleus A and nucleus B in a molecule. The process from which 2D spectra are obtained has four steps.
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Chemical Shift: Internal References and Solvent Effects01:17

Chemical Shift: Internal References and Solvent Effects

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In an NMR sample, precise measurement of the absolute absorption frequencies of nuclei is difficult. A standard internal reference compound is added, and the frequency difference between the reference signal and sample signals is measured.
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2D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)01:19

2D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)

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Heteronuclear single-quantum correlation spectroscopy (HSQC) is a 2D NMR technique that reveals one-bond correlations between hydrogen and a heteronucleus. The HSQC experiment is similar to the heteronuclear correlation experiment (HETCOR) but is more sensitive. In the HSQC spectrum, the proton chemical shift is plotted on the horizontal F2 axis, while the 13C chemical shift is plotted on the vertical F1 axis. The corresponding proton and 13C spectra are also shown. The HSQC contour plot does...
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Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
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High resolution solid-state NMR on the desktop.

Ke Xu1, Fettah Aldudak2, Oliver Pecher3

  • 1University of Siegen, Faculty IV: School of Science and Technology, Department of Chemistry and Biology, Inorganic Materials Chemistry, Adolf-Reichwein-Str. 2, 57076, Siegen, Germany.

Solid State Nuclear Magnetic Resonance
|July 7, 2023
PubMed
Summary
This summary is machine-generated.

High-resolution solid-state NMR is now possible in low-cost permanent magnets using 3D-printed magic-angle spinning modules. This breakthrough enables detailed analysis of paramagnetic materials without expensive superconducting magnets.

Keywords:
3D printingMagic-angle-spinningNMRSolid-state

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Area of Science:

  • Analytical Chemistry
  • Materials Science
  • Spectroscopy

Background:

  • High-resolution nuclear magnetic resonance (NMR) spectroscopy is crucial for characterizing liquid compounds due to the affordability of permanent magnets.
  • Solid-state NMR has been limited to low-resolution analyses of static samples due to space constraints in low-field magnets.

Purpose of the Study:

  • To develop a method for achieving high-resolution solid-state NMR in low-cost permanent magnets.
  • To enable the analysis of paramagnetic solids using magic-angle spinning (MAS) NMR in low magnetic fields.

Main Methods:

  • Miniaturization of magic-angle spinning modules using 3D printing techniques.
  • Development of a conical rotor design using finite element calculations for high-speed sample spinning (>20 kHz).
  • Testing the setup on various diamagnetic and paramagnetic compounds, including battery materials.

Main Results:

  • Demonstrated the feasibility of high-resolution solid-state NMR in permanent magnets.
  • Achieved high spectral resolution for paramagnetic solids, comparable to early electromagnet experiments but with higher spinning speeds.
  • Validated the technique on diverse sample types, including paramagnetic battery materials.

Conclusions:

  • High-resolution low-field magic-angle-spinning NMR is achievable without superconducting magnets.
  • This advancement makes high-resolution solid-state NMR of paramagnetic compounds practical.
  • Potential to establish low-field solid-state NMR as a routine analytical tool for abundant nuclei.