Chemical Analysis of Fluorobenzenes via Multinuclear Detection in the Strong Heteronuclear <i>J</i>-Coupling Regime
Chemical analysis via nuclear magnetic resonance (NMR) spectroscopy using permanent magnets, rather than superconducting magnets, is a rapidly developing field. Performing the NMR measurement in the strong heteronuclear <i>J</i>-coupling regime has shown considerable promise for the chem...
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MDPI AG
2020-05-01
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| Series: | Applied Sciences |
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| author | Derrick C. Kaseman Michael T. Janicke Rachel K. Frankle Tammie Nelson Gary Angles-Tamayo Rami J. Batrice Per E. Magnelind Michelle A. Espy Robert F. Williams |
| author_facet | Derrick C. Kaseman Michael T. Janicke Rachel K. Frankle Tammie Nelson Gary Angles-Tamayo Rami J. Batrice Per E. Magnelind Michelle A. Espy Robert F. Williams |
| author_sort | Derrick C. Kaseman |
| collection | DOAJ |
| description | Chemical analysis via nuclear magnetic resonance (NMR) spectroscopy using permanent magnets, rather than superconducting magnets, is a rapidly developing field. Performing the NMR measurement in the strong heteronuclear <i>J</i>-coupling regime has shown considerable promise for the chemical analysis of small molecules. Typically, the condition for the strong heteronuclear <i>J</i>-coupling regime is satisfied at µT magnetic field strengths and enables high resolution <i>J</i>-coupled spectra (JCS) to be acquired. However, the JCS response to systematic chemical structural changes has largely not been investigated. In this report, we investigate the JCS of C<sub>6</sub>H<sub>6−<i>x</i></sub>F<i><sub>x</sub></i> (<i>x</i> = 0, 1, 2, …, 6) fluorobenzene compounds via simultaneous excitation and detection of <sup>19</sup>F and <sup>1</sup>H at 51.5 µT. The results demonstrate that JCS are quantitative, and the common NMR observables, including Larmor frequency, heteronuclear and homonuclear <i>J</i>-couplings, relative signs of the J-coupling, chemical shift, and relaxation, are all measurable and are differentiable between molecules at low magnetic fields. The results, corroborated by <i>ab initio</i> calculations, provide new insights into the impact of chemical structure and their corresponding spin systems on JCS. In several instances, the JCS provided more chemical information than traditional high field NMR, demonstrating that JCS can be used for robust chemical analysis. |
| first_indexed | 2024-03-10T19:28:43Z |
| format | Article |
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| issn | 2076-3417 |
| language | English |
| last_indexed | 2024-03-10T19:28:43Z |
| publishDate | 2020-05-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Applied Sciences |
| spelling | doaj.art-6d1fb696fed94908bf850d39d107c3ce2023-11-20T02:22:16ZengMDPI AGApplied Sciences2076-34172020-05-011011383610.3390/app10113836Chemical Analysis of Fluorobenzenes via Multinuclear Detection in the Strong Heteronuclear <i>J</i>-Coupling RegimeDerrick C. Kaseman0Michael T. Janicke1Rachel K. Frankle2Tammie Nelson3Gary Angles-Tamayo4Rami J. Batrice5Per E. Magnelind6Michelle A. Espy7Robert F. Williams8Bioenergy and Biome Sciences Group, Los Alamos National Laboratory, Los Alamos, NM 87545, USAInorganic, Isotope, and Actinide Chemistry Group, Los Alamos National Laboratory, Los Alamos, NM 87545, USABioenergy and Biome Sciences Group, Los Alamos National Laboratory, Los Alamos, NM 87545, USAPhysics and Chemistry of Materials Group, Los Alamos National Laboratory, Los Alamos, NM 87545, USAPhysics and Chemistry of Materials Group, Los Alamos National Laboratory, Los Alamos, NM 87545, USAInorganic, Isotope, and Actinide Chemistry Group, Los Alamos National Laboratory, Los Alamos, NM 87545, USAQuantum Group, Los Alamos National Laboratory, Los Alamos, NM 87545, USANon-Destructive Testing and Evaluation Group, Los Alamos National Laboratory, Los Alamos, NM 87545, USABioenergy and Biome Sciences Group, Los Alamos National Laboratory, Los Alamos, NM 87545, USAChemical analysis via nuclear magnetic resonance (NMR) spectroscopy using permanent magnets, rather than superconducting magnets, is a rapidly developing field. Performing the NMR measurement in the strong heteronuclear <i>J</i>-coupling regime has shown considerable promise for the chemical analysis of small molecules. Typically, the condition for the strong heteronuclear <i>J</i>-coupling regime is satisfied at µT magnetic field strengths and enables high resolution <i>J</i>-coupled spectra (JCS) to be acquired. However, the JCS response to systematic chemical structural changes has largely not been investigated. In this report, we investigate the JCS of C<sub>6</sub>H<sub>6−<i>x</i></sub>F<i><sub>x</sub></i> (<i>x</i> = 0, 1, 2, …, 6) fluorobenzene compounds via simultaneous excitation and detection of <sup>19</sup>F and <sup>1</sup>H at 51.5 µT. The results demonstrate that JCS are quantitative, and the common NMR observables, including Larmor frequency, heteronuclear and homonuclear <i>J</i>-couplings, relative signs of the J-coupling, chemical shift, and relaxation, are all measurable and are differentiable between molecules at low magnetic fields. The results, corroborated by <i>ab initio</i> calculations, provide new insights into the impact of chemical structure and their corresponding spin systems on JCS. In several instances, the JCS provided more chemical information than traditional high field NMR, demonstrating that JCS can be used for robust chemical analysis.https://www.mdpi.com/2076-3417/10/11/3836low field NMR<i>J</i>-coupled spectroscopystrong-heteronuclear <i>J</i>-coupling regimefluorobenzenePople notationstrong coupling |
| spellingShingle | Derrick C. Kaseman Michael T. Janicke Rachel K. Frankle Tammie Nelson Gary Angles-Tamayo Rami J. Batrice Per E. Magnelind Michelle A. Espy Robert F. Williams Chemical Analysis of Fluorobenzenes via Multinuclear Detection in the Strong Heteronuclear <i>J</i>-Coupling Regime Applied Sciences low field NMR <i>J</i>-coupled spectroscopy strong-heteronuclear <i>J</i>-coupling regime fluorobenzene Pople notation strong coupling |
| title | Chemical Analysis of Fluorobenzenes via Multinuclear Detection in the Strong Heteronuclear <i>J</i>-Coupling Regime |
| title_full | Chemical Analysis of Fluorobenzenes via Multinuclear Detection in the Strong Heteronuclear <i>J</i>-Coupling Regime |
| title_fullStr | Chemical Analysis of Fluorobenzenes via Multinuclear Detection in the Strong Heteronuclear <i>J</i>-Coupling Regime |
| title_full_unstemmed | Chemical Analysis of Fluorobenzenes via Multinuclear Detection in the Strong Heteronuclear <i>J</i>-Coupling Regime |
| title_short | Chemical Analysis of Fluorobenzenes via Multinuclear Detection in the Strong Heteronuclear <i>J</i>-Coupling Regime |
| title_sort | chemical analysis of fluorobenzenes via multinuclear detection in the strong heteronuclear i j i coupling regime |
| topic | low field NMR <i>J</i>-coupled spectroscopy strong-heteronuclear <i>J</i>-coupling regime fluorobenzene Pople notation strong coupling |
| url | https://www.mdpi.com/2076-3417/10/11/3836 |
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