This
two-dimensional absolute-value HET2DJ spectrum shows (decoupled) 13C
chemical shifts on one 2D axis and 13C-1H coupling
constants on the other 2D axis. Before setting up the HET2DJ experiment, see Acquiring
and Processing 2D Experiments. See the Varian Guide to NMR
Experiments for a complete description of this experiment.
1.
Join the experiment in which the 13C reference spectrum was
collected. Type het2dj.
2.
Type dg. Adjust the parameters listed below for the standard HET2DJ:
·
sfrq=set
by spectrometer
·
tn=’C13’
·
at
= set by spectrometer
·
np=2048
·
sw = sw from 13C reference spectrum
·
ss=2
·
tpwr = listed at console
·
pw = 13C 90° pulse width
·
pp = 1H decoupler 90° pulse width (from shim sheet)
·
pplvl= 1H decoupler pulse power (from shim sheet)
·
d1 = 1H relaxation delay (1-2 * 1H T1)
or ~1.5
·
d2=0
·
tof = tof from 13C reference spectrum
·
nt = multiple of 16
·
ct
= set by computer
·
dn=’H1’
·
dof = tof from 1H reference spectrum
·
dm=’ynny’
·
dmm=’wcw’
·
dmf=9468
·
dpwr= 35
·
sw1 = C-H coupling (~ 200)
·
ni = set using time for experiment (see table below)
·
dp=’y’
·
hs=’nn’
·
reffrq=reffrq from 13C reference spectrum
·
wp1=sw1
·
sp1= -sw1/2
·
temp = 25 su
***TURN OFF THE SPINNER***
Change ni, nt, and d1
to suit your scheduled time.
The
vertical (non-acquisition) resolution equals sw1/ni. Typical values are listed
below for sw1=25000:
|
d1 |
ni |
sw1 |
nt |
time |
vert. res |
d1 |
ni |
sw1 |
nt |
time |
vert. res |
|
1.5 |
32 |
128 |
16 |
0:14 |
4.0 Hz |
1.5 |
32 |
128 |
64 |
0:57 |
4.0 Hz |
|
1.5 |
96 |
128 |
16 |
0:49 |
1.33 |
1.5 |
96 |
128 |
64 |
3:17 |
1.33 |
|
1.5 |
192 |
128 |
16 |
1:58 |
0.67 |
1.5 |
192 |
128 |
64 |
7:51 |
0.67 |
|
1.5 |
32 |
512 |
16 |
0:13 |
16.0 |
1.5 |
32 |
512 |
64 |
0:54 |
16.0 |
|
1.5 |
96 |
512 |
16 |
0:42 |
5.33 |
1.5 |
96 |
512 |
64 |
2:49 |
5.33 |
|
1.5 |
192 |
512 |
16 |
1:29 |
1.50 |
1.5 |
192 |
512 |
64 |
5:56 |
1.50 |
3.
Make sure the spinner is off, then type au to start experiment.
Processing, Displaying, and Plotting:
Process using the procedure for Processing
a 2D Absolute-Value Experiment. Plot Pos. only contours.