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Pulse Sequence

Operation Procedure:

  1. Use HXY probe, install C13-N15 insert for 1H-13C-15N  operation.

See attached pictures

  1. Install the probe and load the shim file.
  1. Install filters and preamplifiers. N15 (60MHz) C13 (150MHz)

C13 channel filter (C13 pass and N15 stop)

See attached pictures

  1. 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

  1. Use zg to calibrate proton 90 degree pulse. Make sure set the center frequency to the peak to be calibrated.
  1. Use cp.av to calibrate CPMAS for C13. Optimize cp.av for the sample.
  1. Use zg or hpdec to find the power level for an exact N15 180 degree pulse.
  1. 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.

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Last updated: 03/17/03.