90O Pulse Width Determination
Optimum data quality in many NMR experiments depends on properly
adjusted pulse duration (or width). There is a linear relationship between pulse
duration and magnetization flip angle so that once one knows the flip angle
that results from a given pulse width one can then readily determine flip angles
produced by other pulse widths. A typical value for the 90° pulse width is around
10 us. The 180° pulse width will be twice the value of the 90° pulse. One can
observe all the pulse width values in an experiment by entering
dps
on the command line to graphically display the pulse sequence. To find the correct
value for the 90° pulse width do the following:
Load a standard 1D parameter set. Set
pw=5
Collect and process a spectrum and adjust the spectrum phase so that all peaks
are symmetric and all peak intensity is above the baseline (ie. do a normal
phase adjustment)
Enter the following:
array (Enter pw for the parameter to be arrayed, 25 for
the number of steps, 2 for the starting value, and 2 for the step
increment)
d1=10
nt=1
go
After acquistion completion enter
wft
to process all the spectra in the array. Enter
dssh
to display all the spectra in the array. It's probably best to zoom in on a
particular peak before doing this, otherwise the entire spectrum is shown as
it varies with pulse width. The first place where the peaks are nulled out is
the 180° pulse. Half of this value (i.e., where the peak intensity is
maximized) is the value for the 90° pulse. Enter
da
to display the array of pw values. Observe the array of spectra and determine
the array index for the first null (the array index is obtained by counting
spectra from left to right). Look at the array of pulse width values and read
the value associated with the array index of the first null, that value is the
180° pulse width. Divide the 180° pulse width by two to obtain the 90° pulse
width.