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

Journal Article · 30 May 2020 · International Journal of Molecular Sciences (Online)

DOI: https://doi.org/10.3390/ijms21113938 · OSTI ID:1631470

Walder, Brennan J. ^[1];

^[1]

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

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.

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

Sponsoring Organization:: USDOE National Nuclear Security Administration (NNSA)

Grant/Contract Number:: AC04-94AL85000

OSTI ID:: 1631470

Alternate ID(s):: OSTI ID: 1634806

Report Number(s):: SAND2020-5728J; IJMCFK; 686478

Journal Information:: International Journal of Molecular Sciences (Online), Vol. 21, Issue 11; ISSN 1422-0067

Publisher:: MDPICopyright Statement

Country of Publication:: United States

Language:: English

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