207Pb chemical shift thermometer at high temperature for magic angle spinning experiments.

Area of Science:

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

Background:

• Accurate temperature calibration is crucial for reproducible and reliable Magic Angle Spinning Nuclear Magnetic Resonance (MAS NMR) experiments.
• Existing temperature calibration methods may have limitations in certain temperature ranges or require specialized equipment.

Purpose of the Study:

• To investigate the temperature dependence of the 207Pb chemical shift in lead nitrate (Pb(NO3)2) MAS NMR spectra.
• To evaluate the feasibility of using this temperature dependence as a sensitive method for sample temperature calibration in MAS NMR.

Main Methods:

• Acquisition of 207Pb MAS NMR spectra of lead nitrate (Pb(NO3)2) at various controlled temperatures.
• Analysis of the temperature-dependent chemical shift of the 207Pb signal.
• Evaluation of NMR sensitivity and line width as a function of temperature.

Main Results:

• A uniform and reproducible temperature dependence of the 207Pb chemical shift was observed in the temperature range of 30 to 400 degrees C.
• The NMR sensitivity and line width remained favorable across the studied temperature range, indicating good signal quality.
• The observed chemical shift variation provides a sensitive probe for temperature determination.

Conclusions:

• The temperature dependence of the 207Pb chemical shift in Pb(NO3)2 MAS NMR is a highly effective and sensitive method for calibrating sample temperatures.
• This method is suitable for a broad temperature range relevant to many solid-state NMR studies.
• Lead nitrate serves as a reliable solid-state NMR thermometer for MAS NMR applications.