Tailoring NMR Experiments for Oriented Samples
Separated local field experiments
A. Free-induction decay

B. Spin Exchange


Lee Goldburg condition

Anatomy of the PISEMA sequence
- Cross Polarization transfer
- Flip H magnetization to magic angle
- Allow 1H/15N to spin-exchange
- Acquire 15N under 1H decoupling


Setup PISEMA step-by-step
- Find the 1H resonance frequency
- Measure the 1H nutation frequency
- Find the Hartmann-Hahn match at off-resonance condition
- Find the phase of the 35.7o pulse
Find the Hartmann-Hahn condition at on-resonance condition
- Adjust X channel power level to match the 1H channel power


Find the 1H resonance frequency
•- - Turn the decoupler power way down
•Sweep the 1H irradiation frequency


Measure the 1H nutation frequency
•-Initial pulse rise time prevent accurate nutation
frequency measurement
•Use pre Spin-lock pulse to accurate measure
1H nutation
frequency



Find the Hartmann-Hahn condition at off-resonance condition
•Require phase-continuous frequency switching
•Match the X channel to
1H
channel during the offset irradiation (+Df)
•Match the X channel to
1H
channel during the offset irradiation (-Df)
•Precede with spin-lock pulse
•No compensation pulse


Find the phase of the 35.7o pulse


Typical PISEMA spectra
•The line width (FWHH) is <200 Hz typical for
single-crystal

Hardware requirement
1. DDS (direct digital synthesizer)
2. Or use small angle phase shifter (PMLG: phase-modulated Lee-Goldburg)
B. Proton / X channel amplifier
1. Frequent phase inversion may overwhelm protection circuit
C. Probe tuning
1. use directional coupler to monitor the reflective power
2. Triple frequency tuning
3. Steady-state tuning
A.

B.


