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Updated: Aug 6, 2026
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Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
Published on: September 17, 2017
13C solid-state NMR chemical shift reproducibility across spectrometers
Erika Bartůňková1, Jan Blahut2, Renée Siegel3
1Institute of Organic Chemistry and Biochemistry, Czech Academy of Sciences, Flemingovo nám. 2, Prague, 160 00, Czech Republic; Department of Analytical Chemistry, Faculty of Sciences, Charles University, Hlavova 8, Prague, 128 00, Czech Republic.
Solid State Nuclear Magnetic Resonance
|July 23, 2026
Summary
Solid-state 13C NMR chemical shifts are highly reproducible across different instruments and field strengths. Consistent referencing ensures reliable data for aggregated chemical shift databases.
Area of Science:
- Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy.
- Materials science and chemistry.
Background:
- Solid-state NMR is crucial for characterizing crystalline materials, including pharmaceuticals.
- Reproducibility of chemical shift measurements across different instruments is essential for data aggregation and comparative studies.
Purpose of the Study:
- To evaluate the reproducibility of precise 13C NMR chemical shifts across multiple solid-state NMR instruments.
- To assess the impact of varying magnetic field strengths and MAS rates on measurement consistency.
Main Methods:
- Measurements of 13C NMR chemical shifts were performed on five different solid-state NMR instruments using a set of five reference compounds.
- All instruments were calibrated using a common referencing protocol with an internal DSS standard.
- Data were analyzed to determine variations in isotropic shifts across instruments and conditions.
Main Results:
- Excellent agreement in 13C isotropic shifts was observed across all instruments, with typical variations within 0.2 ppm.
- No significant systematic dependence of chemical shifts on magnetic field strength (300-1000 MHz) or MAS rate was found.
- Error analysis confirmed the robustness of measured shifts, with discrepancies generally within tenths of a ppm.
Conclusions:
- Solid-state 13C NMR chemical shifts demonstrate high reproducibility when a consistent referencing protocol is applied.
- These findings support the reliability of chemical shift databases compiled from multiple laboratories and instruments.
- The results lend confidence to multi-instrument studies and the use of aggregated solid-state NMR data.
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