Protecting air/moisture-sensitive samples using perdeuterated paraffin wax for solid-state NMR experiments under magic-angle spinning.
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| Title: | Protecting air/moisture-sensitive samples using perdeuterated paraffin wax for solid-state NMR experiments under magic-angle spinning. |
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| Authors: | Foley, Emma A.1 (AUTHOR), Thuma, Joseph F.1 (AUTHOR), Mayer, Jacob1,2 (AUTHOR), Halder, Mita2 (AUTHOR), Huang, Wenyu1 (AUTHOR), Perras, Frédéric A.1,2 (AUTHOR), Culver, Damien B.2 (AUTHOR), Kobayashi, Takeshi1,2 (AUTHOR) takeshi@iastate.edu |
| Source: | Journal of Magnetic Resonance. Oct2025, Vol. 379, pN.PAG-N.PAG. 1p. |
| Subjects: | Magic angle spinning, Paraffin wax, Organometallic compounds, Spin exchange, Nuclear magnetic resonance |
| Abstract: | Solid-state nuclear magnetic resonance (SSNMR) spectroscopy is a powerful technique for materials characterization, yet its application to air- and moisture-sensitive materials is often hindered by the difficulty in maintaining an inert environment during magic-angle spinning (MAS). This is particularly true for fast-MAS rotors that do not generally provide tight seals. Herein, we present a generalizable approach employing perdeuterated paraffin waxes— n -icosane-d42 and c -dodecane-d24—as protective embedding media to analyze sensitive organometallic catalysts using SSNMR. We demonstrate that these waxes significantly slow oxidative degradation under MAS conditions. Weak background 1H and 13C NMR signals from the waxes are effectively suppressed using double-quantum filtration and cross-polarization techniques. These findings offer a robust method for expanding the scope of SSNMR to air-sensitive systems, with implications for the structural study of reactive materials and catalysts. [Display omitted] • Protection air/moisture-sensitive samples using perdeuterated paraffin waxes is demonstrated for fast-MAS experiments. • 1H and 13C NMR signals from the matrix are readily eliminated using double-quantum filtering or cross-polarization. • This approach offers a valuable framework to facilitate SSNMR characterization of systems not fully compatible with MAS. [ABSTRACT FROM AUTHOR] |
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| Database: | Engineering Source |
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