Nuclear Magnetic Resonance (NMR)

NMR Capabilities

The NMR Service at Loughborough offers liquid and solid-state 500 MHz NMR capabilities for 1D and 2D analysis of small molecules, polymers and solid materials such as zeolites and catalysts. All data will be processed and presented to your requirements.

Instrumentation

JEOL ECZ-500 500MHz instrument with 5mm ROYALPROBE HFX liquid probe and 3.2mm HXMAS solid state probe

1D experiments

1H and 19F on high-frequency coil, with a tuneable low-frequency coil to any nucleus frequency between 31P and 15N – typically used for 13C, 31P 29Si, 27Al, 11B.

A dual-tune mode is available for the high-frequency coil allowing us to carry out proton measurements with fluorine decoupling or vice versa. Furthermore, we can decouple both proton and fluorine simultaneously for 13C spectra, simplifying assignments of 13C spectra of more complex fluorine containing compounds, or allowing C-F DEPT experiments.

For polymeric samples, T2-filtered experiments can allow analysis of end-groups and residual monomers.

1D NOESY/TOCSY/EXSY

2D Experiments

The standard suite of H-X (X typically 13C, 15N) correlation experiments is available for full characterisation– COSY, HMBC, HMQC, NOESY/ROESY, TOCSY for full characterisations.

For polymeric samples and complex mixtures, 1D & 2D diffusion measurements (DOSY) are available, allowing measurement of diffusion coefficients, estimation of molecular weight distribution, and potentially identification of mixtures.

Our HXMAS solid state probe uses 3.2mm solid sample rotors, which are capable of magic-angle spinning (MAS) up to 22 KHz. Approximately 100 mg of sample is required, however the technique is non-destructive.

1D experiments

Simple MAS experiments for 1H and 19F available in single-tune mode, with a tuneable low frequency coil typically used for X = 13C, 31P, 29Si, 27Al, 23Na, 7Li, 79Br, 35Cl.

Cross-polarisation experiments for enhancement of sensitivity of nuclei such as 13C, 15N is available for molecules with protons adjacent to the nuclei of interest.

2D experiments

HETCOR (for H-X heteronuclear correlation) and INADEQUATE (for homonuclear) characterisations are available to be discussed on request.

nmr unit

Are you interested in using this facility?

If you are interested in using equipment would like further information please do not hesitate to get in touch.