Articles | Volume 6, issue 2
https://doi.org/10.5194/mr-6-173-2025
© Author(s) 2025. This work is distributed under
the Creative Commons Attribution 4.0 License.
the Creative Commons Attribution 4.0 License.
https://doi.org/10.5194/mr-6-173-2025
© Author(s) 2025. This work is distributed under
the Creative Commons Attribution 4.0 License.
the Creative Commons Attribution 4.0 License.
Coherence locking in a parallel nuclear magnetic resonance probe defends against gradient field spillover
Mengjia He
Institute of Microstructure Technology, Karlsruhe Institute of Technology, Eggenstein-Leopoldshafen, Germany
Neil MacKinnon
CORRESPONDING AUTHOR
Institute of Microstructure Technology, Karlsruhe Institute of Technology, Eggenstein-Leopoldshafen, Germany
Dominique Buyens
Institute of Microstructure Technology, Karlsruhe Institute of Technology, Eggenstein-Leopoldshafen, Germany
Burkhard Luy
Institute for Biological Interfaces 4 – Magnetic Resonance, Karlsruhe Institute of Technology, Eggenstein-Leopoldshafen, Germany
Institute of Organic Chemistry, Karlsruhe Institute of Technology, Karlsruhe, Germany
Institute of Microstructure Technology, Karlsruhe Institute of Technology, Eggenstein-Leopoldshafen, Germany
Related authors
No articles found.
Paul Jelden, Magnus Dam, Jens Hänisch, Martin Börner, Sören Lehmkuhl, Bernhard Holtzapfel, Tabea Arndt, and Jan Gerrit Korvink
Magn. Reson. Discuss., https://doi.org/10.5194/mr-2025-10, https://doi.org/10.5194/mr-2025-10, 2025
Preprint under review for MR
Short summary
Short summary
High critical field superconductors are less sensitive to magnet quenching, providing even higher fields. They can be cooled using cryogens like Helium, but simply using an oscillating pressure field. Using solar or wind energy, the cheap cooling promises magnetic resonance at high field, low operating cost, and renewable energy. Such magnets, made compact, can be used to prepolarise chemical samples, to be analysed in benchtop NMR systems, with better nuclear magnetic resonance spectra.
Sagar Wadhwa, Nan Wang, Klaus-Martin Reichert, Manuel Butzer, Omar Nassar, Mazin Jouda, Jan G. Korvink, Ulrich Gengenbach, Dario Mager, and Martin Ungerer
Magn. Reson., 6, 199–210, https://doi.org/10.5194/mr-6-199-2025, https://doi.org/10.5194/mr-6-199-2025, 2025
Short summary
Short summary
We present a technology that allows for the direct writing of conductive tracks on cylindrical substrates as receiver coils for magnetic resonance (MR) experiments. The structures are written with high precision, which has two benefits. First, the real structures behave very similarly to the simulated designs, reducing the component variation; second, this allows for the writing of coils apart from the fairly straightforward solenoidal coils, thereby making complex designs available for MR microcoils.
Jan Korvink
Magn. Reson. Discuss., https://doi.org/10.5194/mr-2022-24, https://doi.org/10.5194/mr-2022-24, 2023
Publication in MR not foreseen
Short summary
Short summary
The magic angle spinning (MAS) technique of solid state NMR requires samples to be rapidly rotated within a magnetic field. The rotation rate speed record is 150 kHz, or 9 million RPM, and hence MAS turbines hold the world rotation speed record for extended objects. The containers holding the samples are made of the strongest materials known, to be able to withstand the excessive centrifugal forces. To overcome the speed limit, this paper delineates a way to do so using an optical tweezers setup
Jens D. Haller, David L. Goodwin, and Burkhard Luy
Magn. Reson., 3, 53–63, https://doi.org/10.5194/mr-3-53-2022, https://doi.org/10.5194/mr-3-53-2022, 2022
Short summary
Short summary
In contrast to adiabatic excitation, recently introduced SORDOR-90 pulses provide effective transverse 90° rotations throughout their bandwidth, with a quadratic offset dependence of the phase in the x,y plane. Together with phase-matched SORDOR-180 pulses, this enables a direct implementation of the Böhlen–Bodenhausen approach for frequency-swept pulses for a type of 90°/180° pulse–delay sequence. Example pulse shapes are characterised, and an application is given with a 19F-PROJECT experiment.
Neil MacKinnon, Mehrdad Alinaghian, Pedro Silva, Thomas Gloge, Burkhard Luy, Mazin Jouda, and Jan G. Korvink
Magn. Reson., 2, 835–842, https://doi.org/10.5194/mr-2-835-2021, https://doi.org/10.5194/mr-2-835-2021, 2021
Short summary
Short summary
To increase experimental efficiency, information can be encoded in parallel by taking advantage of highly resolved NMR spectra. Here we demonstrate parallel encoding of optimal diffusion parameters by selectively using a resonance for each molecule in the sample. This yields a factor of n decrease in experimental time since n experiments can be encoded into a single measurement. This principle can be extended to additional experimental parameters as a means to further improve measurement time.
Cyril Charlier, Neil Cox, Sophie Martine Prud'homme, Alain Geffard, Jean-Marc Nuzillard, Burkhard Luy, and Guy Lippens
Magn. Reson., 2, 619–627, https://doi.org/10.5194/mr-2-619-2021, https://doi.org/10.5194/mr-2-619-2021, 2021
Short summary
Short summary
The HSQC experiment developed by Bodenhausen and Ruben is a cornerstone for modern NMR. When used in the field of metabolomics, the common practice of decoupling in the proton dimension limits the acquisition time and hence the resolution. Here, we present a virtual decoupling method to maintain both spectral simplicity and resolution, and demonstrate how it increases information content with the zebra mussel metabolome as an example.
Pedro Freire Silva, Mazin Jouda, and Jan G. Korvink
Magn. Reson., 2, 607–617, https://doi.org/10.5194/mr-2-607-2021, https://doi.org/10.5194/mr-2-607-2021, 2021
Short summary
Short summary
We use the theory of magnetostatic reciprocity to compute manufacturable solutions of complex magnet geometries, establishing a quantitative metric for the placement and subsequent orientation of discrete pieces of permanent magnetic material. This leads to self-assembled micro-magnets, adjustable magnetic arrays, and an unbounded magnetic field intensity in a small volume, despite realistic modelling of complex material behaviours.
Sagar Wadhwa, Mazin Jouda, Yongbo Deng, Omar Nassar, Dario Mager, and Jan G. Korvink
Magn. Reson., 1, 225–236, https://doi.org/10.5194/mr-1-225-2020, https://doi.org/10.5194/mr-1-225-2020, 2020
Short summary
Short summary
Magnetic resonance detectors require a high degree of precision to be useful. Their design must e.g. carefully weigh field strength and field homogeneity to find the best compromise. Here we show that inverse computational design is a viable method to find such a
trade-off. Apart from the electromagnetic field solution, the simulation program also determines the boundary between insulating and conducting material and moves the material boundaries around until the compromise is best satisfied.
Mazin Jouda, Saraí M. Torres Delgado, Mehrdad Alinaghian Jouzdani, Dario Mager, and Jan G. Korvink
Magn. Reson., 1, 105–113, https://doi.org/10.5194/mr-1-105-2020, https://doi.org/10.5194/mr-1-105-2020, 2020
Short summary
Short summary
We have assembled a few off-the-shelf electronic chips and a popular Arduino Uno microcomputer board in an automatic system that performs so-called tuning and matching of an arbitrary NMR probe head at very low cost. This removes the tedium of doing the job by hand, the bane of many NMR analysts. It also brings accuracy and repeatability into the process, which is so necessary for high throughput analysis or when working with low-field permanent magnesystems with excessive magnetic field drift.
Related subject area
Field: Liquid-state NMR | Topic: Instrumentation
A fast sample shuttle to couple high and low magnetic fields. Applications to high-resolution relaxometry
Workflow for systematic design of electrochemical in operando NMR cells by matching B0 and B1 field simulations with experiments
A portable NMR platform with arbitrary phase control and temperature compensation
Magnetostatic reciprocity for MR magnet design
An electrochemical cell for in operando 13C nuclear magnetic resonance investigations of carbon dioxide/carbonate processes in aqueous solution
Overhauser dynamic nuclear polarization (ODNP)-enhanced two-dimensional proton NMR spectroscopy at low magnetic fields
ArduiTaM: accurate and inexpensive NMR auto tune and match system
Jorge A. Villanueva-Garibay, Andreas Tilch, Ana Paula Aguilar Alva, Guillaume Bouvignies, Frank Engelke, Fabien Ferrage, Agnes Glémot, Ulric B. le Paige, Giulia Licciardi, Claudio Luchinat, Giacomo Parigi, Philippe Pelupessy, Enrico Ravera, Alessandro Ruda, Lucas Siemons, Olof Stenström, and Jean-Max Tyburn
Magn. Reson. Discuss., https://doi.org/10.5194/mr-2024-25, https://doi.org/10.5194/mr-2024-25, 2025
Revised manuscript accepted for MR
Short summary
Short summary
Investigating NMR phenomena at variable magnetic fields is useful and insightful, in particular for hyperpolarization and molecular dynamics. To benefit from high-resolution at high magnetic fields, field-dependent investigations can be performed on a high-field NMR spectrometer, using a sample shuttle apparatus for field cycling. Here we introduce a new design of sample shuttle, which is fast, reliable, and narrow. We show a series of applications to small molecules and a protein in solution.
Michael Schatz, Matthias Streun, Sven Jovanovic, Rüdiger-A. Eichel, and Josef Granwehr
Magn. Reson., 5, 167–180, https://doi.org/10.5194/mr-5-167-2024, https://doi.org/10.5194/mr-5-167-2024, 2024
Short summary
Short summary
We developed a workflow using finite element methods to optimise electrochemical cell designs for in operando nuclear magnetic resonance by accurately matching magnetic field and radio frequency field simulations with experimental data. Guidelines for enhanced sensitivity and field homogeneity are given. A radio frequency amplification effect in coin cells is described by empirical formulae, which have the potential to improve spatial selectivity in future in operando applications.
Qing Yang, Jianyu Zhao, Frederik Dreyer, Daniel Krüger, and Jens Anders
Magn. Reson., 3, 77–90, https://doi.org/10.5194/mr-3-77-2022, https://doi.org/10.5194/mr-3-77-2022, 2022
Short summary
Short summary
We have presented a CMOS-based NMR platform featuring arbitrary phase control and coherent detection in a non-zero intermediate frequency (IF) receiver architecture as well as active automatic temperature compensation. The proposed platform is centered around a custom-designed NMR-on-a-chip transceiver. The entire system achieves a phase stability well below 1° in consecutive pulse acquire experiments and keeps a normalized standard deviation in the measured T2 values of 0.45 % over 100 min.
Pedro Freire Silva, Mazin Jouda, and Jan G. Korvink
Magn. Reson., 2, 607–617, https://doi.org/10.5194/mr-2-607-2021, https://doi.org/10.5194/mr-2-607-2021, 2021
Short summary
Short summary
We use the theory of magnetostatic reciprocity to compute manufacturable solutions of complex magnet geometries, establishing a quantitative metric for the placement and subsequent orientation of discrete pieces of permanent magnetic material. This leads to self-assembled micro-magnets, adjustable magnetic arrays, and an unbounded magnetic field intensity in a small volume, despite realistic modelling of complex material behaviours.
Sven Jovanovic, P. Philipp M. Schleker, Matthias Streun, Steffen Merz, Peter Jakes, Michael Schatz, Rüdiger-A. Eichel, and Josef Granwehr
Magn. Reson., 2, 265–280, https://doi.org/10.5194/mr-2-265-2021, https://doi.org/10.5194/mr-2-265-2021, 2021
Short summary
Short summary
This work presents a setup for the investigation of electrochemical processes during operation (in operando) using nuclear magnetic resonance (NMR) spectroscopy. The setup was designed to minimize the interferences between the NMR instrument and the electrochemical equipment. Employing this setup, the dynamic equilibrium of carbon dioxide in aqueous bicarbonate electrolyte has been monitored in operando, revealing intercations with the electrode setup.
Timothy J. Keller and Thorsten Maly
Magn. Reson., 2, 117–128, https://doi.org/10.5194/mr-2-117-2021, https://doi.org/10.5194/mr-2-117-2021, 2021
Short summary
Short summary
Typically, low-field Overhauser dynamic nuclear polarization (ODNP) experiments are 1D NMR experiments to study hydration dynamics. Here, we demonstrate the application of ODNP-enhanced 2D J-resolved (JRES) spectroscopy to improve spectral resolution beyond the limit imposed by the line broadening introduced by the paramagnetic polarizing agent. Crucial to these experiments is interleaved spectral referencing to compensate for temperature-induced field drifts over the course of the experiment.
Mazin Jouda, Saraí M. Torres Delgado, Mehrdad Alinaghian Jouzdani, Dario Mager, and Jan G. Korvink
Magn. Reson., 1, 105–113, https://doi.org/10.5194/mr-1-105-2020, https://doi.org/10.5194/mr-1-105-2020, 2020
Short summary
Short summary
We have assembled a few off-the-shelf electronic chips and a popular Arduino Uno microcomputer board in an automatic system that performs so-called tuning and matching of an arbitrary NMR probe head at very low cost. This removes the tedium of doing the job by hand, the bane of many NMR analysts. It also brings accuracy and repeatability into the process, which is so necessary for high throughput analysis or when working with low-field permanent magnesystems with excessive magnetic field drift.
Cited articles
Barskiy, D. A., Salnikov, O. G., Romanov, A. S., Feldman, M. A., Coffey, A. M., Kovtunov, K. V., Koptyug, I. V., and Chekmenev, E. Y.: NMR Spin-Lock Induced Crossing (SLIC) Dispersion and Long-Lived Spin States of Gaseous Propane at Low Magnetic Field (0.05T), J. Magn. Reson., 276, 78–85, https://doi.org/10.1016/j.jmr.2017.01.014, 2017. a
Becker, M., Cheng, Y.-T., Voigt, A., Chenakkara, A., He, M., Lehmkuhl, S., Jouda, M., and Korvink, J. G.: Artificial Intelligence-Driven Shimming for Parallel High Field Nuclear Magnetic Resonance, Sci. Rep., 13, 17983, https://doi.org/10.1038/s41598-023-45021-6, 2023. a
Cheng, Y.-T., Jouda, M., and Korvink, J.: Sample-Centred Shimming Enables Independent Parallel NMR Detection, Sci. Rep., 12, 14149, https://doi.org/10.1038/s41598-022-17694-y, 2022. a
Ciobanu, L., Jayawickrama, D. A., Zhang, X., Webb, A. G., and Sweedler, J. V.: Measuring Reaction Kinetics by Using Multiple Microcoil NMR Spectroscopy, Angew. Chem. Int. Ed., 42, 4669–4672, https://doi.org/10.1002/anie.200351901, 2003. a
COMSOL AB: COMSOL Multiphysics® Version 6.1, https://www.comsol.com (last access: 25 September 2024), 2022. a
DeVience, S. J., Walsworth, R. L., and Rosen, M. S.: Nuclear Spin Singlet States as a Contrast Mechanism for NMR Spectroscopy, NMR Biomed., 26, 1204–1212, https://doi.org/10.1002/nbm.2936, 2013a. a
DeVience, S. J., Walsworth, R. L., and Rosen, M. S.: Preparation of Nuclear Spin Singlet States Using Spin-Lock Induced Crossing, Phys. Rev. Lett., 111, 173002, https://doi.org/10.1103/PhysRevLett.111.173002, 2013b. a
DeVience, S. J., Walsworth, R. L., and Rosen, M. S.: Probing Scalar Coupling Differences via Long-Lived Singlet States, J. Magn. Reson., 262, 5761, https://doi.org/10.1016/j.jmr.2015.12.003, 2015. a
DeVience, S. J., Greer, M., Mandal, S., and Rosen, M. S.: Homonuclear J-Coupling Spectroscopy at Low Magnetic Fields Using Spin-Lock Induced Crossing**, Chem. Phys. Chem., 22, 2128–2137, https://doi.org/10.1002/cphc.202100162, 2021. a
Gram, M., Seethaler, M., Gensler, D., Oberberger, J., Jakob, P. M., and Nordbeck, P.: Balanced Spin-Lock Preparation for B1-Insensitive and B0-Insensitive Quantification of the Rotating Frame Relaxation Time T1ρ, Magn. Reson. Med., 85, 2771–2780, https://doi.org/10.1002/mrm.28585, 2021. a
Grzesiek, S. and Bax, A.: Spin-Locked Multiple Quantum Coherence for Signal Enhancement in Heteronuclear Multidimensional NMR Experiments, J. Biomol. NMR, 6, 335–339, https://doi.org/10.1007/BF00197815, 1995. a
He, M., Faderl, D., MacKinnon, N., Cheng, Y.-T., Buyens, D., Jouda, M., Luy, B., and Korvink, J. G.: A Digital Twin for Parallel Liquid-State Nuclear Magnetic Resonance Spectroscopy, Commun. Eng., 3, 1–13, https://doi.org/10.1038/s44172-024-00233-0, 2024. a, b
He, M., MacKinnon, N., Buyens, D., Luy, B., and Korvink, J. G.: Coherence locking in a parallel NMR probe defends against gradient field spillover, Zenodo [code and data set], https://doi.org/10.5281/zenodo.15188023, 2025. a
Hogben, H. J., Krzystyniak, M., Charnock, G. T., Hore, P. J., and Kuprov, I.: Spinach–a Software Library for Simulation of Spin Dynamics in Large Spin Systems, J. Magn. Reson., 208, 179–194, https://doi.org/10.1016/j.jmr.2010.11.008, 2011. a
Holz, M. and Weingartner, H.: Calibration in Accurate Spin-Echo Self-Diffusion Measurements Using 1H and Less-Common Nuclei, J. Magn. Res. (1969), 92, 115–125, https://doi.org/10.1016/0022-2364(91)90252-O, 1991. a
Hou, T., MacNamara, E., and Raftery, D.: NMR Analysis of Multiple Samples Using Parallel Coils: Improved Performance Using Reference Deconvolution and Multidimensional Methods, Anal. Chim. Acta, 400, 297–305, https://doi.org/10.1016/S0003-2670(99)00706-0, 1999. a
Jiang, B. and Chen, W.: On-Resonance and off-Resonance Continuous Wave Constant Amplitude Spin-Lock and T1ρ Quantification in the Presence of B1 and B0 Inhomogeneities, NMR Biomed., 31, e3928, https://doi.org/10.1002/nbm.3928, 2018. a
Kim, Y., Liu, M., and Hilty, C.: Parallelized Ligand Screening Using Dissolution Dynamic Nuclear Polarization, Anal. Chem., 88, 11178–11183, https://doi.org/10.1021/acs.analchem.6b03382, 2016. a
Kovtunov, K. V., Truong, M. L., Barskiy, D. A., Koptyug, I. V., Coffey, A. M., Waddell, K. W., and Chekmenev, E. Y.: Long-Lived Spin States for Low-Field Hyperpolarized Gas MRI, Chem. – Eur. J., 20, 14629–14632, https://doi.org/10.1002/chem.201405063, 2014. a
Kupče, Ē., Frydman, L., Webb, A. G., Yong, J. R. J., and Claridge, T. D. W.: Parallel Nuclear Magnetic Resonance Spectroscopy, Nat. Rev. Methods Primers, 1, 1–23, https://doi.org/10.1038/s43586-021-00024-3, 2021. a
Lei, K.-M., Ha, D., Song, Y.-Q., Westervelt, R. M., Martins, R., Mak, P.-I., and Ham, D.: Portable NMR with Parallelism, Anal. Chem., 92, 2112–2120, https://doi.org/10.1021/acs.analchem.9b04633, 2020. a
LeMaster, D. M. and Richards, F. M.: Proton-nitrogen-15 heteronuclear NMR studies of Escherichia coli thioredoxin in samples isotopically labeled by residue type, Biochemistry, 24, 7263–7268, 1985. a
Li, Y., Wolters, A. M., Malawey, P. V., Sweedler, J. V., and Webb, A. G.: Multiple Solenoidal Microcoil Probes for High-Sensitivity, High-Throughput Nuclear Magnetic Resonance Spectroscopy, Anal. Chem., 71, 4815–4820, https://doi.org/10.1021/ac990855y, 1999. a
Liu, Y. and Prestegard, J. H.: Measurement of one and two bond N–C couplings in large proteins by TROSY-based J-modulation experiments, J. Magn. Reson., 200, 109–118, 2009. a
MacNamara, E., Hou, T., Fisher, G., Williams, S., and Raftery, D.: Multiplex Sample NMR: An Approach to High-Throughput NMR Using a Parallel Coil Probe, Anal. Chim. Acta, 397, 9–16, https://doi.org/10.1016/S0003-2670(99)00387-6, 1999. a, b
Rodin, B. A., Kiryutin, A. S., Yurkovskaya, A. V., Ivanov, K. L., Yamamoto, S., Sato, K., and Takui, T.: Using Optimal Control Methods with Constraints to Generate Singlet States in NMR, J. Magn. Reson., 291, 14–22, https://doi.org/10.1016/j.jmr.2018.03.005, 2018. a
Ross, A., Schlotterbeck, G., Senn, H., and von Kienlin, M.: Application of Chemical Shift Imaging for Simultaneous and Fast Acquisition of NMR Spectra on Multiple Samples, Angew. Chem. Int. Ed., 40, 3243–3245, https://doi.org/10.1002/1521-3773(20010903)40:17<3243::AID-ANIE3243>3.0.CO;2-F, 2001. a
Sonnefeld, A., Razanahoera, A., Pelupessy, P., Bodenhausen, G., and Sheberstov, K.: Long-Lived States of Methylene Protons in Achiral Molecules, Sci. Adv., 8, eade2113, https://doi.org/10.1126/sciadv.ade2113, 2022. a
Stejskal, E. O. and Tanner, J. E.: Spin Diffusion Measurements: Spin Echoes in the Presence of a Time-Dependent Field Gradient, J. Chem. Phys., 42, 288–292, https://doi.org/10.1063/1.1695690, 1965. a
The MathWorks, Inc.: MATLAB Version R2023b, The MathWorks, Inc., https://www.mathworks.com/products/matlab.html (last access: 31 March 2025), 2023. a
Wang, H., Ciobanu, L., Edison, A. S., and Webb, A. G.: An Eight-Coil High-Frequency Probehead Design for High-Throughput Nuclear Magnetic Resonance Spectroscopy, J. Magn. Reson., 170, 206–12, https://doi.org/10.1016/j.jmr.2004.07.001, 2004. a
Waugh, J. S.: Theory of Broadband Spin Decoupling, J. Magn. Reson., 50, 30–49, https://doi.org/10.1016/0022-2364(82)90029-4, 1982. a
Short summary
Parallel NMR (nuclear magnetic resonance) detection enhances measurement throughput for high-throughput screening. However, local gradients in parallel detectors cause field spillover in adjacent channels, leading to spin dephasing and signal loss. This study introduces a compensation scheme using optimized pulses to mitigate gradient-induced field inhomogeneity through coherence locking. The proposed approach offers an effective solution for NMR probes with parallel, independently switchable gradient coils.
Parallel NMR (nuclear magnetic resonance) detection enhances measurement throughput for...