Varian UNITY INOVA NMR, Установка оборудования, Страница: 25 / 65

Chapter 3. CP/MAS Solids Module Installation
24
UNITY
INOVA Solids Hardware Installation 01-999044-00 C0501
6. Record a pair of
13
C spectra by entering
dof=50000, –50000 ga
(see Figure
2 ).
7. Measure the residual splitting of the dioxane triplet. Use
h2cal
to calculate
γ
B
2
.
Minimum values are shown in Table 1 .
Set
level2
to achieve a
γ
B
2
as close to these minimum values as possible. Do not
exceed this power level for any other experiment. Note this value.
8. If the probe does not make specification, check for rf losses in the decoupler circuitry
going to the probe.
ACQUISITION SAMPLE PROCESSING FLAGS
sfrq 100.57 date April 1 lb 10.00 il n
tn C13 file exp sb not used toss n
at 0.100 DECOUPLING gf not used pdp n
np 6016 dn H1 awc not used dp y
sw 3000.0 dof arrayed lsfid not used SPECIAL
xpol n dm nny phfid not used srate 415
tpwr 55 dmm c wtfile temp not used
tpwrf 51 dpwr 63 proc ft
pw 8.0 level1 57 fn 32768
p1 0 level1f 200
d1 10.000 level2 63
tof 0 level2f 4095 werr
nt 1 wexp
ct 1 wbs
wnt
FLAGS
ai no ph
Gamma-H2 calculation
See J. Magnetic Resonance 7:442 (1972)
jo = 284.00 Hz, dof[1] = –50000.00 Hz, dof[2] = 50000.00 Hz
jr[1] = 165.00 Hz, jr[2] = 167.00 Hz
Gamma-H2 = 69404.97 Hz
90 degree pulse = 3.6 usec
coalescence frequency = –457.51 Hz
Figure 2. Decoupler Field
γ
B
2
Table 1. Maximum
γ
B
2
Values
Magnet
Varian RT Probe,
7mm Varian VT Probe,
7mm Doty Probe, 7mm
HS
Other Probes
200 MHz 75 kHz — 60 kHz See individual
specs
300 MHz 75 kHz 80 kHz 60 kHz
400 MHz 60 kHz 70 kHz 55 kHz