Agilent Technologies VARIAN Dual, Руководство пользователя, Страница: 22 / 30

01-999124-00 J 0606 Dual and Dual Broadband NMR Probes Installation
21
Testing Probes on MERCURYplus
13
C Lineshape Test
1. Enter
rtp('/vnmr/tests/C13res') su
.
2. Tune the probe.
3. Enter
nt=4 lb='n' dmm='c' d1=60 su
.
4. Set the sample spinning rate at 20
±
5 Hz.
5. Enter
ga
to acquire the spectrum.
6. Plot the spectrum using
wp=50
and use
dres
to determine the linewidth at 50% of
the decoupled peak.
7. Do the following if decoupling is not complete:
a. Obtain a proton spectrum in a different experiment.
b. Set the cursor at the center of the single peak
c. Enter
movetof
d. Enter
tof?
to display the new values of
tof
.
e. Record the value.
8. Enter
jexp
n, where n is the experiment number of the carbon experiment
(e.g.,
jexp2
to join experiment
2
).
9. Set
dof
to the value of
tof
obtained in the proton spectrum.
10. Repeat step 5 .
11. Write the results for each probe in the forms provided in Test Results, page 27 .
1
H Observe 90° Pulse Width
This procedure calibrates
tpwr
and the 90° pulse width for
1
H.
1. Open GLIDE by clicking the GLIDE button in the VNMR menu.
2. Click on the Setup icon.
3. Insert the sample in the magnet using the Insert button in the Setup window.
4. Select Calibrate Proton from the Experiment drop-down menu.
Do not need to select a solvent.
5. Turn off autolock and autoshim if the system is locked and shimmed on the sample.
6. Click the Setup button at the bottom of the Setup window.
7. Tune the probe.
8. Click on the Acquire button under Custom.
9. Enter an appropriate value for
pwmax
.
10. Click on Close at the bottom of the Acquire window.
11. Click the Go icon in the GLIDE window.
A plot of arrayed spectra is produced.
12. Write the results for each probe in the forms provided in Test Results, page 27 .