Operation Procedure:
- Use HXY probe, install C13-N15 insert for 1H-13C-15N
operation.
See attached pictures
- Install the probe and load the shim file.
- Install filters and preamplifiers. N15 (60MHz) C13
(150MHz)
C13 channel filter (C13 pass and
N15 stop)
See attached pictures
- Tune all three channels for the test sample. Load
REDORsetup program
And then type ii to initialize the
hardware. Type edasp to display the hardware links. 1H
à 1000Watts; 13C
à 1000Watts; and 15N
à 500 Watts.
From Two channel to three channel
conversion: for C13 Tune, CCW 180
degree and match CCW two turns. All three channels should be well tuned with the
sample
- Use zg to calibrate proton 90 degree pulse. Make sure
set the center frequency to the peak to be calibrated.
- Use cp.av to calibrate CPMAS for C13. Optimize cp.av for
the sample.
- Use zg or hpdec to find the power level for an exact N15
180 degree pulse.
- Use cpredxy8.av to check the signal of C13 with/without
N15 180 pulse. With N15 180 pulse, the signal should be smaller, about 10%.
9. Use cpredxy2d.av for 2D. ds=4 td 2048, si 8k. Use QF on F2; qsim on
F1. type expt for current experiment time.