小中大共享:去偶道中氢的90度脉宽的测定(pp)
Determining the 1H 90° pulse width of the decoupler
It is strongly recommended that you use the 90% CHCL3 in d6-acetone sample for this calibration, since this sample has strong carbon signals that may be detected with a small number of transients (nt).
Click on main menu, setup, 13C Acetone to select carbon standard parameters.
Type ppcal to set up the pp calibration experiment.
Adjust the following parameters: pp=0
pplvl=49 WARNING!!! Do NOT set pplvl larger than 49!
d1=3.0
d2=0.003185 for the acetone standard. Set to 1/(2*JCH)
pw=13C 90° pulse width
p1=13C 180° pulse width
dm='yny'
dmm='wcw'
dof =-426.0
nt=4 for the acetone standard
gain='n'
Type ga and phase the spectrum.
Type gain='y'
Set pp to your estimate of the decoupler 90° pulse width
Type ga
Repeat steps 6 and 7 until the intensity of the chloroform peak is minimum (zero intensity is ideal).