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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.
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]
Copyright of Journal of Magnetic Resonance is the property of Academic Press Inc. and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)
Database: Engineering Source
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Header DbId: egs
DbLabel: Engineering Source
An: 187664430
AccessLevel: 6
PubType: Academic Journal
PubTypeId: academicJournal
PreciseRelevancyScore: 0
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  Label: Title
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  Data: Protecting air/moisture-sensitive samples using perdeuterated paraffin wax for solid-state NMR experiments under magic-angle spinning.
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  Data: <searchLink fieldCode="AR" term="%22Foley%2C+Emma+A%2E%22">Foley, Emma A.</searchLink><relatesTo>1</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Thuma%2C+Joseph+F%2E%22">Thuma, Joseph F.</searchLink><relatesTo>1</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Mayer%2C+Jacob%22">Mayer, Jacob</searchLink><relatesTo>1,2</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Halder%2C+Mita%22">Halder, Mita</searchLink><relatesTo>2</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Huang%2C+Wenyu%22">Huang, Wenyu</searchLink><relatesTo>1</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Perras%2C+Frédéric+A%2E%22">Perras, Frédéric A.</searchLink><relatesTo>1,2</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Culver%2C+Damien+B%2E%22">Culver, Damien B.</searchLink><relatesTo>2</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Kobayashi%2C+Takeshi%22">Kobayashi, Takeshi</searchLink><relatesTo>1,2</relatesTo> (AUTHOR)<i> takeshi@iastate.edu</i>
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  Data: <searchLink fieldCode="JN" term="%22Journal+of+Magnetic+Resonance%22">Journal of Magnetic Resonance</searchLink>. Oct2025, Vol. 379, pN.PAG-N.PAG. 1p.
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  Data: <searchLink fieldCode="DE" term="%22Magic+angle+spinning%22">Magic angle spinning</searchLink><br /><searchLink fieldCode="DE" term="%22Paraffin+wax%22">Paraffin wax</searchLink><br /><searchLink fieldCode="DE" term="%22Organometallic+compounds%22">Organometallic compounds</searchLink><br /><searchLink fieldCode="DE" term="%22Spin+exchange%22">Spin exchange</searchLink><br /><searchLink fieldCode="DE" term="%22Nuclear+magnetic+resonance%22">Nuclear magnetic resonance</searchLink>
– Name: Abstract
  Label: Abstract
  Group: Ab
  Data: 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]
– Name: AbstractSuppliedCopyright
  Label:
  Group: Ab
  Data: <i>Copyright of Journal of Magnetic Resonance is the property of Academic Press Inc. and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract.</i> (Copyright applies to all Abstracts.)
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RecordInfo BibRecord:
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      – Type: doi
        Value: 10.1016/j.jmr.2025.107935
    Languages:
      – Code: eng
        Text: English
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        PageCount: 1
        StartPage: N.PAG
    Subjects:
      – SubjectFull: Magic angle spinning
        Type: general
      – SubjectFull: Paraffin wax
        Type: general
      – SubjectFull: Organometallic compounds
        Type: general
      – SubjectFull: Spin exchange
        Type: general
      – SubjectFull: Nuclear magnetic resonance
        Type: general
    Titles:
      – TitleFull: Protecting air/moisture-sensitive samples using perdeuterated paraffin wax for solid-state NMR experiments under magic-angle spinning.
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            NameFull: Foley, Emma A.
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            NameFull: Thuma, Joseph F.
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            NameFull: Mayer, Jacob
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            NameFull: Huang, Wenyu
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            – D: 01
              M: 10
              Text: Oct2025
              Type: published
              Y: 2025
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              Value: 379
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            – TitleFull: Journal of Magnetic Resonance
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