Performing VT experiments on 500MHz DMX spectrometer.
The case of higher than ambient temperature.
* Use the proper spinner turbine for VT experiments. Actually,
the gray fiber glass spinners
are design for VT experiments.
* Make sure that the VT nitrogen gas is hooked up to the
glass Dewar in the probe and that
gas is flowing. The glass Dewar is very fragile,
please take extremely cautions while
working with it. The flow rate should be
~500 l/h.
* Turn “ON” the VT controller
on spectrometer’s console.
* While in xwinnmr software type ‘
EDTE ’ command and EDTE main window appears.
* Make sure that target sample temperature is set up to
room temperature.
* Using EDTE menu set the maximum
heater power to 15%. It is rather rare that a
higher
value will be needed.
* Make sure that your target temperature does not exceed
the limit of the probe
specifications. Exceeding the probe’s limit temperature
will damage the probe. Magnet
might also be damaged.
* Set the temperature 5 degree higher
than present and turn the heater button ‘ON’.
The
button is placed on the spectrometer’s console.
Another heater button “ON/OFF” that is
placed in the EDTE
menu is not designed to work.
* Wait until sample temperature is close to target and increase
it another 5 degrees.
* To get to the final required temperature, proceed in the
steps of no more than 5 degrees to
avoid thermal and current shock in the hardware.
* When the temperature has been achieved wait a certain
period of time before you start to
perform NMR experiment to equalize the temperature
across the sample. A 20 –30
minute period of time is usually needed.
However, you may like to find out your own
waiting time for temperature equalization.
* After experiment is finished, decrease the temperature
in the 5degree intervals until the
room temperature is achieved. Never introduce the
thermal shock to the system by
changing the temperature with too large intervals.
* Turn off the heater by pushing the button heater “
Off” on VT controller.
* Exit the EDTE menu.
*To cool down probe’s electronic and shims to the ambient conditions
an additional
time between 30–120 minutes
is needed. This depend on how long experiment
took place and what was the final temperature. Mark
your VT experiment in
logbook so a next user will be aware about previous conditions.
Consider those
limitation while signing up so the sign up policy will
be obeyed.
*To find out more details, please refer to the Bruker manual
that is available in
NMR laboratory.
The case of lower than ambient temperature
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