This is an inversion recovery experiment to measure direct detect T1. The experiment is pseudo 2D. This is NYSBC standard data set and pulse program for 1H-13C cross polarization with rotor synchronized 13C hahnecho followed by 13C acquisition with 1H decoupling. The pulse program has power safety limitations specific for the particular probe. The pulse program T1ir_3.2EF750.nysbc, ramp shape file tancn_100_SCALE and include file power_intro.incl are located in the dataset directory.
To minimized heating of conductive samples, we recommend using an Efree/lowE probe. However, a combination of frictional heating from spinning and RF heating on long pulses on both channel may cause substantial sample heating and temperature gradient across the sample even in an Efree probe. The heating may damage the sample. The heating and temperature gradient across the rotor may substantially compromise the precision of measurements and data fitting.
[https://www.ncbi.nlm.nih.gov/pubmed/10868566?dopt=Abstract] Heating of samples induced by fast magic-angle spinning, Brus, J., Solid State Nucl. Magn. Reson. 16, 151–160 (2000).
[https://onlinelibrary.wiley.com/doi/abs/10.1002/mrc.4450] Heating and temperature gradients of lipid bilayer samples induced by RF irradiation in MAS solid-state NMR experiments, Wang, J., Zhang, Z., Zhao, W., Wang, L. & Yang, J., Magn. Reson. Chem. 54, 753–759 (2016).
[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
R1ρ experiments require long simultaneous medium to high power pulses on 1H and X channels. Make sure that you don't exceed the maximum allowed powers/lengths and damage the probe. When in doubt, contact the manufacturer.
Make sure that recycle delay is longer than 3xT1
The experiments were performed with crystallized u-15N,13C-labeled-N-acetyl-valine
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 use a monoexponential function to obtain T1 values