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Here is an overview of the whole system. From front to back we have a computer that controls
everything, a large console that houses most of the electrical components. The 11.7 Tesla magnet is the large
"tin can" in the background. The samples are placed in a probe within the magnet. The probe is attached to
console by a number of cables.
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Here are the tubes that hold the samples. These 5 mm tubes are 8 inches tall and require
a volume of about 0.5 ml. Other sized tubes are used, for example we also use 10 mm tubes.
NMR is a relatively insensitive technique so the concentration of the sample needs to be high as
possible. One rule of thumb is that your generic protein should be at soluble to at least 0.5 mM.
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The sample drops into the magnet on a cushion of air through the orange tube at the top. The sample tube
drops into the probe which is centered in the coils of superconducting wire that produce the magnetic
field. The superconduting wire is kept in a bath of liquid helium (-269 C) so that it has no resistance
to current. The liquid helium bath is kept cold by a dewar of liquid nitrogen (-196 C). You can see the ice
build up on the rubber tubes at the top of magnet where the liquid nitrogen boils off. The whole magnet is
isolated from the building by the three black vibration isolation colums at the bottom.
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Here is Jon Vural dropping an NMR sample into the probe. Note that he has attached a "spinner" to the tube
so that it fits into the bore of the magnet correctly. Don't forget the spinner!
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Here Jon is holding a broad band probe that he is about to install into the bottom of the magnet.
The small box on the floor at the left with the green lights is a preamplifier that is also useful
for tuning and matching the inductance of the probe with that of the cables and console to ensure that
maximum amount of power reaches the sample.
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Here is what a probe looks like once it is installed. There is not all that
much to see since most of the probe in contained within the magnet. All that is left outside are the cable
connections and the tuning and matching devices.
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Here is a close up of the external region of our broad band probe. On the left are the bnc cable
connectors to attach the probe to the preamplifer and console. On the right is a glass bulb connector
that attaches to a hose that carries an air stream cooled by a cooling unit. This allows the temperature
of the sample to be carefully regulated. The gold sliders with the numbers are used to tune and match
this probe for each sample and each type of nucleus.
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This is the main console with the doors open. This is the proverbial "guts of the machine." Each component
has a specific role. In the next few frames we'll explain a few of them.
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This is the gradient controler. In conjunction with an amplifier (out of view on top of the console) the
gradient controller allows us to rapidly and reproducibly apply a magnetic gradient to the sample. This
is extremely useful for selecting coherences and water suppression. It also makes shimming the magnet
(to produce a homogeneous field around the sample) a snap.
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This unit houses a series of control boards and acts as the console's brain.
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This is the frequency generator. It produces a very pure frequency that can later be modifed
to correspond to the frequencies of each nucleus.
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This unit controls the shims. The shims are extra coils that surround the probe. By adjusting
the current in the shim coils the magnetic field around the sample can be made more homogeneous.
Shimming is somewhat analogous to adding wedges (shims) around a door or window to insure it's level,
hence the term shimming.
Good shims are essential for narrow lineshapes and good water suppression.
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A variable temperature unit is essential to regulate the temperature of the sample in the probe.
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Two components here actually. On the left is the unit that modifies the pure frequency from the
frequency generator to produce the actual frequencies that will be sent to the transmitters and
ultimately the probe. On the right is a digitizer that collects the signal from the probe after a pulse.
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This is the acquistion controller. It routes signals to and from the probe.
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Finally we get to the three transmitters on this spectrometer. The center
transmitter is dedicated to 1H signals while the top and bottom can be tuned to a variety of
nuclei. Typically, we use them for 13C, 15N, and 31P.
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Here I am at the computer. From here your can contol the whole beast (except for tuning adjustments
which must be done at the probe). Experiments can be set up and run and the collected data processed using
the Bruker software. However, we do most of our processing and analysis at other workstations so we can
keep the spectrometer running full tilt. Note that I'm signing the log book. Always sign the logbook!
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