Quantification of Uncoupled Spin Domains in Spin-Abundant Disordered Solids

Walder, Brennan J.; Alam, Todd M.

doi:10.3390/ijms21113938

Title: Quantification of Uncoupled Spin Domains in Spin-Abundant Disordered Solids

Abstract

Materials often contain minor heterogeneous phases that are difficult to characterize yet nonetheless significantly influence important properties. Here we describe a solid-state NMR strategy for quantifying minor heterogenous sample regions containing dilute, essentially uncoupled nuclei in materials where the remaining nuclei experience heteronuclear dipolar couplings. NMR signals from the coupled nuclei are dephased while NMR signals from the uncoupled nuclei can be amplified by one or two orders of magnitude using Carr-Meiboom-Purcell-Gill (CPMG) acquisition. The signal amplification by CPMG can be estimated allowing the concentration of the uncoupled spin regions to be determined even when direct observation of the uncoupled spin NMR signal in a single pulse experiment would require an impractically long duration of signal averaging. We use this method to quantify residual graphitic carbon using 13 C CPMG NMR in poly(carbon monofluoride) samples synthesized by direct fluorination of carbon from various sources. Our detection limit for graphitic carbon in these materials is better than 0.05 mol%. The accuracy of the method is discussed and comparisons to other methods are drawn.

Authors:

Walder, Brennan J.;

Publication Date:: 2020-05-30

Research Org.:: Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

Sponsoring Org.:: USDOE National Nuclear Security Administration (NNSA)

OSTI Identifier:: 1631470

Alternate Identifier(s):: OSTI ID: 1634806

Report Number(s):: SAND2020-5728J
Journal ID: ISSN 1422-0067; IJMCFK; PII: ijms21113938

Grant/Contract Number:: AC04-94AL85000

Resource Type:: Published Article

Journal Name:: International Journal of Molecular Sciences (Online)

Additional Journal Information:: Journal Name: International Journal of Molecular Sciences (Online) Journal Volume: 21 Journal Issue: 11; Journal ID: ISSN 1422-0067

Publisher:: MDPI

Country of Publication:: Switzerland

Language:: English

Subject:: 36 MATERIALS SCIENCE

Citation Formats


                    Walder, Brennan J., and Alam, Todd M. Quantification of Uncoupled Spin Domains in Spin-Abundant Disordered Solids.  Switzerland: N. p., 2020. 
        Web.  doi:10.3390/ijms21113938.

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                    Walder, Brennan J., & Alam, Todd M. Quantification of Uncoupled Spin Domains in Spin-Abundant Disordered Solids.  Switzerland.  doi:https://doi.org/10.3390/ijms21113938

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                    Walder, Brennan J., and Alam, Todd M. Sat .  
        "Quantification of Uncoupled Spin Domains in Spin-Abundant Disordered Solids".  Switzerland.  doi:https://doi.org/10.3390/ijms21113938.

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@article{osti_1631470,

  title        = {Quantification of Uncoupled Spin Domains in Spin-Abundant Disordered Solids},

  author       = {Walder, Brennan J. and Alam, Todd M.},

  abstractNote = {Materials often contain minor heterogeneous phases that are difficult to characterize yet nonetheless significantly influence important properties. Here we describe a solid-state NMR strategy for quantifying minor heterogenous sample regions containing dilute, essentially uncoupled nuclei in materials where the remaining nuclei experience heteronuclear dipolar couplings. NMR signals from the coupled nuclei are dephased while NMR signals from the uncoupled nuclei can be amplified by one or two orders of magnitude using Carr-Meiboom-Purcell-Gill (CPMG) acquisition. The signal amplification by CPMG can be estimated allowing the concentration of the uncoupled spin regions to be determined even when direct observation of the uncoupled spin NMR signal in a single pulse experiment would require an impractically long duration of signal averaging. We use this method to quantify residual graphitic carbon using 13 C CPMG NMR in poly(carbon monofluoride) samples synthesized by direct fluorination of carbon from various sources. Our detection limit for graphitic carbon in these materials is better than 0.05 mol%. The accuracy of the method is discussed and comparisons to other methods are drawn.},

  doi          = {10.3390/ijms21113938},

  journal      = {International Journal of Molecular Sciences (Online)},

  number       = 11,

  volume       = 21,

  place        = {Switzerland},

  year         = {2020},

  month        = {5}

}

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Title: Quantification of Uncoupled Spin Domains in Spin-Abundant Disordered Solids

Abstract

Citation Formats

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Cooperation between Active Material, Polymeric Binder and Conductive Carbon Additive in Lithium Ion Battery Cathode
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Practical guides for x-ray photoelectron spectroscopy: First steps in planning, conducting, and reporting XPS measurements
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QCPMG-MAS NMR of Half-Integer Quadrupolar Nuclei
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On paramagnetism in fluorinated graphite: EPR and solid state NMR study
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EPR and Solid-State NMR Studies of Poly(dicarbon monofluoride) (C ₂ F) _n
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Quantitative Characterization of Humic Substances by Solid-State Carbon-13 Nuclear Magnetic Resonance
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NMR in rotating solids
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29Si and 17O (Q)CPMG-MAS solid-state NMR experiments as an optimum approach for half-integer nuclei having long T1 relaxation times
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A material science perspective of pharmaceutical solids
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Spatial heterogeneity as the structure feature for structure–property relationship of metallic glasses
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Quantitative cross-polarization NMR spectroscopy in uniformly 13C-labeled solids
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Increased 29Si NMR sensitivity in glasses with a Carr–Purcell–Meiboom–Gill echotrain
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Further conventions for NMR shielding and chemical shifts IUPAC recommendations 2008
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High Frequency Dynamic Nuclear Polarization
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Determination of aromatic hydrocarbon fraction in oil shale by 13C n.m.r. with magic-angle spinning
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Proton‐enhanced NMR of dilute spins in solids
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Nuclear magnetic resonance study of fluorine–graphite intercalation compounds and graphite fluorides
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X-ray diffraction patterns of graphite and turbostratic carbon
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Application of ¹¹⁹ Sn CPMG MAS NMR for Fast Characterization of Sn Sites in Zeolites with Natural ¹¹⁹ Sn Isotope Abundance
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Communication: Phase incremented echo train acquisition in NMR spectroscopy
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Zur Konstitution des Kohlenstoff-Monofluorids
journal, August 1947

Nuclear Spin-Lattice Relaxation Via Paramagnetic Centers Without Spin Diffusion
journal, August 1968

Improved sensitivity and quantification for 29Si NMR experiments on solids using UDEFT (Uniform Driven Equilibrium Fourier Transform)
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Polarization-Enhanced NMR Spectroscopy of Biomolecules in Frozen Solution
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Sensitivity-Enhanced Quadrupolar-Echo NMR of Half-Integer Quadrupolar Nuclei. Magnitudes and Relative Orientation of Chemical Shielding and Quadrupolar Coupling Tensors
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The CPMG Pulse Sequence in Strong Magnetic Field Gradients with Applications to Oil-Well Logging
journal, March 1995

EPR study on petroleum cokes annealed at different temperatures and used in lithium and sodium batteries
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On the interaction of nuclear spins in a crystalline lattice
journal, May 1949

Axiomatic theories of ideal stretched exponential relaxation (SER)
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Symmetry pathways in solid-state NMR
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Study on the Structure of C-S-H Gels of Slag–Cement Hardened Paste by 29Si, 27Al MAS NMR
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Nuclear Spin-Lattice Relaxation via Paramagnetic Centers
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Solid State ¹³ C and ¹⁹ F NMR Characterization of Fluorinated Charcoal
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Categories of Coherence Pathways for the CPMG Sequence
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29Si NMR in solid state with CPMG acquisition under MAS
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Solid-State NMR ( ¹⁹ F and ¹³ C) Study of Graphite Monofluoride (CF) _n : ¹⁹ F Spin−Lattice Magnetic Relaxation and ¹⁹ F/ ¹³ C Distance Determination by Hartmann−Hahn Cross Polarization
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Equivalence of the time-domain matched filter and the spectral-domain matched filter in one-dimensional NMR spectroscopy
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Correlating structural distributions in silica glass with two-dimensional $J$ -resolved spectroscopy
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Characterizing Nonexponential Spin-Lattice Relaxation in Solid-State NMR by Fitting to the Stretched Exponential
journal, January 1995