Lead‐207 NMR spectroscopy at 1.4 T: Application of benchtop instrumentation to a challenging <i>I</i> = ½ nucleus

Bernard, Guy M.; Michaelis, Vladimir K.

doi:10.1002/mrc.5036

Cited by 4 publications

(5 citation statements)

References 55 publications

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“…Besides the experimentally demanding methods previously mentioned, another practically attractive avenue is the development of benchtop, low-magnetic field 207 Pb NMR spectroscopy (with a permanent magnet) for the routine characterization of LHPs, as recently demonstrated for MAPbCl 3 . 284…”

Section: A-cations: Dynamics and Surfacesmentioning

confidence: 99%

“…Although their DNP enhancement factors were moderate for MAPbCl 3 (15–20) and MAPbBr 3 (3 to 4) at the applied magnetic field strength (9.4 T) and negligible for MAPbI 3 , their results showcased a path to the efficient sampling of both LHP thin films and surface species in LHP NCs, which are morphologies with even lower lead concentrations than microcrystalline powders. Besides the experimentally demanding methods previously mentioned, another practically attractive avenue is the development of benchtop, low-magnetic field 207 Pb NMR spectroscopy (with a permanent magnet) for the routine characterization of LHPs, as recently demonstrated for MAPbCl 3 …”

Section: Pb Nmr Spectroscopy Of Lead-halide Perovskitesmentioning

confidence: 99%

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Solid-State NMR and NQR Spectroscopy of Lead-Halide Perovskite Materials

2020

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Two-and three-dimensional lead-halide perovskite (LHP) materials are novel semiconductors that have generated broad interest owing to their outstanding optical and electronic properties. Characterization and understanding of their atomic structure and structure−property relationships are often nontrivial as a result of the vast structural and compositional tunability of LHPs as well as the enhanced structure dynamics as compared with oxide perovskites or more conventional semiconductors. Nuclear magnetic resonance (NMR) spectroscopy contributes to this thrust through its unique capability of sampling chemical bonding element-specifically ( 1/2 H, 13 C, 14/15 N, 35/37 Cl, 39 K, 79/81 Br, 87 Rb, 127 I, 133 Cs, and 207 Pb nuclei) and locally and shedding light onto the connectivity, geometry, topology, and dynamics of bonding. NMR can therefore readily observe phase transitions, evaluate phase purity and compositional and structural disorder, and probe molecular dynamics and ionic motion in diverse forms of LHPs, in which they can be used practically, ranging from bulk single crystals (e.g., in gamma and X-ray detectors) to polycrystalline films (e.g., in photovoltaics, photodetectors, and light-emitting diodes) and colloidal nanocrystals (e.g., in liquid crystal displays and future quantum light sources). Herein we also outline the immense practical potential of nuclear quadrupolar resonance (NQR) spectroscopy for characterizing LHPs, owing to the strong quadrupole moments, good sensitivity, and high natural abundance of several halide nuclei ( 79/81 Br and 127 I) combined with the enhanced electric field gradients around these nuclei existing in LHPs as well as the instrumental simplicity. Strong quadrupole interactions, on one side, make 79/81 Br and 127 I NMR rather impractical but turn NQR into a high-resolution probe of the local structure around halide ions.

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Section: A-cations: Dynamics and Surfacesmentioning

confidence: 99%

Section: Pb Nmr Spectroscopy Of Lead-halide Perovskitesmentioning

confidence: 99%

Solid-State NMR and NQR Spectroscopy of Lead-Halide Perovskite Materials

2020

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“…Finally, other nuclei such as 7 Li in the mining industry [28], 129 Xe in biosensors [29], and 207 Pb in various applications [30], are special to specific areas and may not be as useful for biomedical applications.…”

Section: One-dimensional Benchtop Nmr Spectroscopymentioning

confidence: 99%

Benchtop NMR-Based Metabolomics: First Steps for Biomedical Application

2023

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Nuclear magnetic resonance (NMR)-based metabolomics is a valuable tool for identifying biomarkers and understanding the underlying metabolic changes associated with various diseases. However, the translation of metabolomics analysis to clinical practice has been limited by the high cost and large size of traditional high-resolution NMR spectrometers. Benchtop NMR, a compact and low-cost alternative, offers the potential to overcome these limitations and facilitate the wider use of NMR-based metabolomics in clinical settings. This review summarizes the current state of benchtop NMR for clinical applications where benchtop NMR has demonstrated the ability to reproducibly detect changes in metabolite levels associated with diseases such as type 2 diabetes and tuberculosis. Benchtop NMR has been used to identify metabolic biomarkers in a range of biofluids, including urine, blood plasma and saliva. However, further research is needed to optimize the use of benchtop NMR for clinical applications and to identify additional biomarkers that can be used to monitor and manage a range of diseases. Overall, benchtop NMR has the potential to revolutionize the way metabolomics is used in clinical practice, providing a more accessible and cost-effective way to study metabolism and identify biomarkers for disease diagnosis, prognosis, and treatment.

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“…Current benchtop NMR devices are dedicated to liquid-state samples, and to date, no benchtop spectrometer for solid-state NMR detection -for instance with an option of magic-angle spinning-has been reported. However, Bernard and Michaelis reported 207 Pb spectra of lead salts in a powder form placed inside a benchtop spectrometer, and compared the results to those obtained with a high-field spectrometer [31]. The corresponding spectra (Figure 3) show that chemical shift anisotropy can be detected on a benchtop spectrometer, although the experiment duration -4 days at 1. suppression blocks [32], pure shift [33], ultrafast 2D [34] or diffusion-encoded [35] pulse sequences.…”

Section: Probes and Accessoriesmentioning

confidence: 99%

Recent advances in benchtop NMR spectroscopy and its applications

Castaing‐Cordier

Bouillaud

Farjon

et al. 2021

Annual Reports on NMR Spectroscopy

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Benchtop NMR spectroscopy has known a major growth over the last decade, thanks to the design of permanent, compact magnets in the 1-2 T range, that provide remarkable performance in terms of resolution and sensitivity. Although resulting spectra are more limited than their high-field counterparts, the achievable structural and quantitative information can be maximized by a clever use of pulse sequences -in particular those involving gradient pulses-and by advanced data processing algorithms. In this chapter, we describe the main characteristics of benchtop NMR spectroscopy in 2020, both in terms of hardware and typical performance. We highlight the most recent methodological improvements in the field, in terms of pulse sequences, hyperpolarization and data processing, which have significantly improved the resolution and sensitivity of benchtop NMR spectrometers. Finally, we discuss major applications of benchtop NMR spectroscopy, for reaction and process monitoring, but also for quality control and profiling. The number of papers in this field in the last few years undoubtedly highlights the major role that benchtop NMR has to play for applications in areas such as food and pharmaceutical industry, flow chemistry, and profiling of complex samples.

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Lead‐207 NMR spectroscopy at 1.4 T: Application of benchtop instrumentation to a challenging I = ½ nucleus

Cited by 4 publications

References 55 publications

Solid-State NMR and NQR Spectroscopy of Lead-Halide Perovskite Materials

Solid-State NMR and NQR Spectroscopy of Lead-Halide Perovskite Materials

Benchtop NMR-Based Metabolomics: First Steps for Biomedical Application

Recent advances in benchtop NMR spectroscopy and its applications

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