Agilent Technologies VARIAN Dual, Manual, Page: 16 / 30

01-999124-00 J 0606 Dual and Dual Broadband NMR Probes Installation
15
Testing Probes on VnmrS and
UNITY
INOVA Systems
a. Enter
r1=xx/5
, where
xx
is the specified pw90 specification for the probe.
b. Enter
array('pw',20,r1,r1)
to create a pw array covering
approximately 360 degrees of nutation.
c. Do the following if the sample does not contain
0.2% Cr(acac):
Enter
d1=30 ga
.
14. Enter
dssh
after the last spectrum is obtained.
The
pw
for the first minimum is the 180
°
pulse and the 90
°
pulse is half this value.
15. Write the results for each probe in the forms provided in Test Results, page 27 .
13
C Spinning Resolution & Lineshape
This test measures the 50%, 0.55%, and 0.11% levels of the ASTM sample. This test and
the
13
C spinning sidebands test (the next test) must be passed simultaneously.
1. Insert the ASTM sample in the probe and spin it.
2. Enter
rtp('/vnmr/tests/C13res') su
.
3. Tune the probe.
4. Enter:
• VnmrS and INOVA—
nt=1
.
• Mercury—
nt=4
.
5. Set the decoupler modulation to
dmm='c'
and
d1=60
.
6. Set the sample spinning rate at 20
±
5 Hz.
7. Change the decoupler power:
• VnmrS and INOVA—
dpwr
to 30 to 42 dB
• Mercury—
dpwr
to 3 or 4 dB below the
dpwr
of
γ
H
2
.
8. Array
dof
to set the decoupler frequency on the dioxane
1
H resonance.
To obtain the best possible resolution, it may be necessary to optimize the position
of the decoupler (
dof
) to within 0.4 Hz of the correct frequency.
9. Enter
ga
to acquire the spectrum.
10. Set
dof
to the value that produced the best resolution.
11. Enter
ga
to acquire the spectrum.
12. Plot the spectrum using
wp=50
.
13. Enter
dres
to determine the linewidth at 50% of the decoupled peak.
14. Increase
vs
by 100 times, plot the expanded spectrum, and measure the linewidth at
0.55% and 0.11%.
15. Write the results for each probe in the forms provided in Test Results, page 27 .
16. Continue with
13
C Spinning Sidebands, page 15 .
13
C Spinning Sidebands
This test and the
13
C spinning resolution and lineshape est (the previous test) must be
passed simultaneously.
1. Measure the
13
C spinning sidebands on the same spectrum as
13
C lineshape and
resolution.