SSNMR; 7 mm MAS NMR probe to a single-crystal goniometer

Solid State Nuclear Magnetic Resonance
Volume 30, Issue 1 , July 2006, Pages 55-59

Hardware modification of a 7 mm MAS NMR probe to a single-crystal goniometer

Gábor Kovács and János Rohonczy
Department of General and Inorganic Chemistry, Institute of Chemistry, Eötvös Loránd University, Budapest, Hungary

Abstract

Tensorial terms of the Hamiltonian can be measured by solid-state single-crystal nuclear magnetic resonance (NMR) spectroscopy which requires a goniometer NMR probehead. Goniometer probes; however, are not standard parts of solid NMR spectrometers and are available only at a much higher price than magic-angle spinning (MAS) probeheads widely used in research. Due to requirements of MAS experiments, modern probeheads are designed for small ceramic rotors, which are 1–4 mm in diameter, to reach very high angular frequencies, so there are several older 7 mm MAS probeheads used rarely todays in NMR laboratories. In this paper, a simple method is presented how to rebuild step-by-step a 7 mm Bruker MAS probehead to be suitable for single-crystal spectroscopy. In the second part 31P chemical shift tensors of Na4P2O7·10H2O are determined to demonstrate the functionality of the rebuilt probehead.

Keywords: NMR; Single crystal; MAS probe; ASICS; Goniometer; Sodium pyrophosphate; Home-built probehead; Nuclear magnetic resonance; 31-P NMR; Crystal orientation