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A standard for silver CP/MAS experiments.

Glenn H Penner1, Wenli Li

  • 1Department of Chemistry, University of Guelph, Ont., N1G 2W1, Guelph, Canada. gpenner@uoguelph.ca <gpenner@uoguelph.ca>

Solid State Nuclear Magnetic Resonance
|May 24, 2003
PubMed
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Silver methanesulfonate (AgSO3CH3) is an excellent 109Ag standard for solid-state NMR. Its 109Ag CP/MAS spectrum provides a single, narrow peak, simplifying experimental setup and data analysis.

Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) Spectroscopy
  • Inorganic Chemistry
  • Materials Science

Background:

  • Establishing reliable standards is crucial for accurate solid-state NMR experiments.
  • Silver-109 (109Ag) NMR requires a well-defined and photo-stable standard for chemical shift referencing.
  • Chemical shift tensor parameters provide insights into the local electronic environment of the nucleus.

Purpose of the Study:

  • To evaluate silver methanesulfonate (AgSO3CH3) as a superior 109Ag standard for Cross-Polarization Magic-Angle Spinning (CP/MAS) NMR.
  • To characterize the 109Ag chemical shift and tensor parameters of solid silver methanesulfonate.
  • To correlate NMR findings with the known crystal structure of silver methanesulfonate.

Main Methods:

  • Solid-state 109Ag NMR spectroscopy using CP/MAS techniques.

Related Experiment Videos

  • Acquisition of both magic-angle spinning and static spectra.
  • Determination of 109Ag chemical shift and chemical shift tensor parameters (span and skew).
  • Comparison of experimental data with crystallographic information.

    • Main Results:

    • Silver methanesulfonate exhibits a single, relatively narrow 109Ag CP/MAS peak at moderate spinning speeds.
    • The isotropic 109Ag chemical shift was determined to be 87.2 ppm relative to 9 M aqueous AgNO3.
    • Static spectrum analysis yielded chemical shift tensor components: δ11=191 ppm, δ22=63 ppm, and δ33=8 ppm.
    • Calculated span (Ω) of 183 ppm and skew (κ) of -0.39 are consistent with the crystal structure.

    Conclusions:

    • Silver methanesulfonate is a highly effective and photo-stable 109Ag standard for solid-state NMR.
    • The determined NMR parameters are in excellent agreement with the crystallographic data, validating its use.
    • This compound simplifies 109Ag NMR experiments, offering a reliable reference for chemical shift determination.