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Related Concept Videos

¹H NMR of Conformationally Flexible Molecules: Variable-Temperature NMR01:15

¹H NMR of Conformationally Flexible Molecules: Variable-Temperature NMR

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The axial and equatorial protons in cyclohexane can be distinguished by performing a variable-temperature NMR experiment. In this process, except for one proton, the remaining eleven protons are replaced by deuterium. The deuterium substitution avoids the possible peak splitting caused by the spin-spin coupling between the adjacent protons. The remaining proton flips between the axial and equatorial positions.
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¹H NMR of Conformationally Flexible Molecules: Temporal Resolution00:52

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At room temperature, the chair conformer of cyclohexane undergoes rapid ring flipping between two equivalent chair conformers at a rate of approximately 105 times per second. These two chair conformers are in equilibrium. The rapid ring flipping results in the interconversion of the axial proton to an equatorial proton and an equatorial to the axial proton. Such interconversions are too rapid and cannot be detected on the NMR timescale. Hence, the NMR spectrometer cannot distinguish between the...
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NMR Spectroscopy Of Amines01:19

NMR Spectroscopy Of Amines

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In proton NMR spectroscopy, primary amines and secondary amines showcase their N–H protons as a broad signal in the chemical shift range between δ 0.5 and 5 ppm. The exact position in this range depends on several factors, including sample concentration, hydrogen bonding, and the type of solvent used. Since amine protons undergo fast proton exchange in solution, the protons are labile and therefore do not participate in any splitting with adjacent protons. Thus, the observed peak is...
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¹³C NMR: Distortionless Enhancement by Polarization Transfer (DEPT)01:20

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When proton-coupled carbon-13 spectra are simplified by a broadband proton decoupling technique, structural information about the coupled protons is lost. Distortionless enhancement by polarization transfer (DEPT) is a technique that provides information on the number of hydrogens attached to each carbon in a molecule. While the DEPT experiment utilizes complex pulse sequences, the pulse delay and flip angle are specifically manipulated. The resulting signals have different phases depending on...
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¹³C NMR: ¹H–¹³C Decoupling01:04

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The probability of having two carbon-13 atoms next to each other is negligible because of the low natural abundance of carbon-13. Consequently, peak splitting due to carbon-carbon spin-spin coupling is not observed in spectra. However, protons up to three sigma bonds away split the carbon signal according to the n+1 rule, resulting in complicated spectra.
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2D NMR: Overview of Homonuclear Correlation Techniques01:16

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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.
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Related Experiment Video

Updated: Apr 26, 2026

Rapid Scan Electron Paramagnetic Resonance Opens New Avenues for Imaging Physiologically Important Parameters In Vivo
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Using electron paramagnetic resonance to map N@C₆₀ during high throughput processing.

Simon R Plant1, Kyriakos Porfyrakis

  • 1Department of Materials, University of Oxford, Parks Road, Oxford OX1 3PH, UK. s.r.plant@bham.ac.uk.

The Analyst
|July 24, 2014
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Summary

High-purity nitrogen-vacancy in a C60 fullerene (N@C60) can be achieved using high-performance liquid chromatography (HPLC). This method enables efficient, scalable production of N@C60 for quantum applications.

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Area of Science:

  • Quantum Information Science
  • Materials Science
  • Analytical Chemistry

Background:

  • Endohedral fullerene N@C60 exhibits unique electron spin properties, making it suitable for molecular spin qubits and probes.
  • High-purity N@C60 samples are crucial for advancing its application in quantum technologies.
  • Efficient and scalable production methods are needed to meet the demand for high-purity N@C60.

Purpose of the Study:

  • To investigate high-throughput processing of N@C60 using HPLC for scalable production.
  • To develop a method for determining N@C60 purity and retention time without isolation.
  • To establish an efficient procedure for isolating high-purity N@C60.

Main Methods:

  • High-performance liquid chromatography (HPLC) with high throughput (18 L h⁻¹, 1.5–2 MPa).
  • Detection using electron paramagnetic resonance (EPR) spectroscopy.
  • Chromatogram peak position analysis for retention time and purity determination.

Main Results:

  • HPLC successfully processed N@C60 at high throughput.
  • EPR detection allowed mapping of N@C60 during processing.
  • Retention time and relative purity were determined without isolating N@C60, enabling optimized processing.

Conclusions:

  • A time-efficient, high-throughput HPLC procedure was established for N@C60 enrichment.
  • This method allows for the isolation of high-purity N@C60 samples.
  • The developed technique is key to advancing the use of N@C60 in quantum computing and sensing.