experiment to measure 13C/ T2 in a 1H observe CPHSQC at fast MAS.

This pseudo 2D experiment measures T2 in a 1H observe CP-HSQC at fast MAS (1.3mm probe at 60kHz spinning frequency).

Citation

https://www.ncbi.nlm.nih.gov/pubmed/25102442 E. Barbet-Massin, A.J. Pell, J.S. Retel, et al., Rapid Proton-Detected NMR Assignment for Proteins with Fast Magic Angle Spinning., JACS 136 (35), pp 12489-12497 (2014).

Sample heating

Frictional heating during ultra fast spinning may heat up a sample by up to 40K.

Citation

[https://www.biorxiv.org/content/10.1101/566729v1.full] TmDOTP : An NMR- based Thermometer for Magic Angle Spinning NMR Experiments Dongyu Zhang, Boris Itin, Ann E. McDermott; preprinted

Protocol

Edit a VD list with exponentially increasing rotor synchronized delays.

Samples

The experiments were performed with a precipitated microcrystalline u-13C,15N labeled protein

Processing and analysis

Fourier transform a pseudo-2D experiment in the direct dimension, measure the peak intensities as a function of length of the spin locking pulse and fit it with a monoexponential function. Bruker T1/T2 routine works adequeate for if S/N is high.

Pulse Sequence and Parameter Set