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For a sample that deteriorates, melts, ignites, or explodes when the temperature rises,
decide the setting temperature by taking into consideration the temperature increase
due to spinning.
Tuning after variable temperature
After the sample reaches the measurement temperature, be sure to tune the probe.
When variable temperature (VT) ends
If spinning is stopped or samples are exchanged immediately after VT measurement is
terminated, it will cause a problem. Set the temperature to 30 ℃, stop the spinning after
the probe temperature approaches the room temperature, remove the VT adapter, and then
exchange samples.
3.2
ADJUSTMENT OF MAGIC ANGLE
1.
Insert the standard sample KBr.
2.
Perform spinning.
3.
Set LF channel to Bromine79 observation.
Check that the combination of the stick and the tuning dial is appropriate for the
bromine 79 observation.
4.
Load the pulse sequence mas_adjust_KBr.jxp to the Experiment Tool.
5.
Click the Submit button.
The pulses occur and the measurement starts.
6.
Adjust the phase by the following procedure.
a.
Click the Monitor tab.
The Monitor tab opens.
b.
After selecting the process list in the Processing Preferences panel, click
the Process
c.
Perform the phase adjustment using Phasing Tools.
7.
Adjust the magic angle.
Following the instruction manual for the probe, adjust the magic angle so that the
spinning sideband of KBr becomes the maximum as shown in Figure 3.1.
Fig. 3.1 FID (left) and the spectrum (right) after magic angle adjustment
NMECAXS_V50-SLD-2
button to change the display.
When the Processing Preferences panel does not appear, click the Processing
button on the far right side.
When the Phasing Tools panel does not appear, click the Phasing button on the
far right side.
The magic-angle adjustment mechanism has some backlash of the gears.
Adjust in one direction when fine-tuning.
3 SETTING OF INSTRUMENT CONDITIONS
FT
Spinning sideband
3-3
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