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Nuclear Magnetic Resonance

Spectrocopy: Instrumentation
Cudia, Ignacio, Ugalino
Chem 125
Nuclear spin
Intrinsic property of a particle (in this case, a
nucleus)
Parameterizes the angular momentum
Dependent on the number of protons and
neutrons in the nucleus
Even numbers of both proton and neutron gives
I = 0
Gives rise to the magnetic moment of the
nucleus

Spin quantum number
Nuclear magnetic moment
-Energy levels split due to external magnetic field
-To allow to move from the ground state to the excited state, an energy
equivalent to the difference of the energy level must be applied
-Energy is provided by the Larmor frequency, which is around the
radiofrequency range.


NMR spectroscopy fundamentals
Relaxation of the magnetic moment towards
thermal equilibrium is measured by a
conducting coil, converting the energy to a
electric signal (by Faradays Law of Induction).
In short, when a sample is exposed to a strong,
uniform magnetic field in an NMR expt and is
irradiated with LF, a signal is observed.
For different nuclei, LF is different, thus
produced radiofrequency must be controlled.

FID: Free induction decay
Magnet
consists of a coil of superconducting wire (T < 6 K)
through which current passes
the wire is suspended in a bath of liquid helium
the liquid helium bath is surrounded by a heat shield
kept at 77K
the whole assembly is constructed in a vacuum flask
the bore tube passes through the magnet which is at
room temperature


Shims
shim coils are used to homogenize the
magnetic field
tiny magnetic fields cancel out the small
residual inhomogeneities in the main
magnetic field


Probe
a cylindrical metal tube inserted
into the bore of the magnet

a small coil is used to both excite
and detect the NMR signal

the coil is part of a tuned circuit
consisting of a coil and a
capacitor such that the circuit
they form is resonant at Larmor
frequency


Transmitter
RF source such a frequency
synthesizer

a gate to generate a pulse of RF
energy

an amplifier is used to boost the
small signal to a power of
100W


Receiver
pre-amplifier to boost NMR signal

diplexer to separate receiver and transmitter


Digitizing the signal
ADC converts NMR signal voltage to binary




Digitizing the signal
NO ADC can achieve the Nyquist condition

mixer subtracts frequency to viable levels




low pass filter
mixer
NMR signal
receiver
frequency
Quadrature detection
REFS
http://www.files.chem.vt.edu/chem-
ed/spec/spin/nmr.html
http://upload.wikimedia.org/wikipedia/comm
ons/thumb/3/38/NMR_EPR.gif/300px-
NMR_EPR.gif
Keeler, J. Understanding NMR Spectroscopy.
(2004).