NUCLEAR MAGNETIC RESONANCE

SPECTROSCOPY
1. MEGNET
2. FIELD LOCK
3. SHIM COIL
4. PROBE UNIT
- sample holder
- RF oscillator
- sweep generator
- RF receiver
5. DETECTOR
6. AMPLIFIER & RECORDER
 Magnets produces the magnetic field,
which determines the frequency of any
nucleus.
 Sensitivity and resolution are critically
dependent on quality of magnet.
 It should give homogenous magnetic field,
i.e.the strength of the magnetic field
should not change from point to point.
 The magnet must be capable of producing
a very strong magnetic field with strength
atleast 10,000 gauss.
1. PERMANENT MAGNET

2. ELECTRO MAGNETS

3.SUPER CONDUCTING
MAGNETS
 It is inexpensive and simple to operatre,but it
requires extensive shielding and must be
thermostated.
 They are operated upto 1.9 T.
 They provide field of good homogeneity.
 It provides homogeneous magnetic field at 60-100
MHz.
 This magnetic field is invisible but is responsible for
the most notable property of magnet: a force that
pulls on other ferrromagnetic materials, such as iron,
and attracts or repels other magnet is an object
made from a material that is magnetized and creates
its own persistent magnetic field.
 An everyday example is a refrigerator magnet used to
hold notes on a refrigerator door.
 They require power supply to produce magnetic
field and cooling system to counter the heat
generated from the electric power.
 They are more effective than the permanent
magnet because of possibility of field variation.
 In which the magnetic field is produced by an
electric current , the magnetic field disappears
when the current is turned off.
 Electromagnets usually consist of wire wound in
to a coil.
 A super conducting magnet has an electro
magnet made up of superconducting wire.
 Superconducting wire has a resistance
approximately equal to zero by immersing it in
liquid helium (at 0◦C).
 The length of superconducting wire in the magnet
is typically several miles.
Swipeeng –change change the
magnetic field, frequency,
keep constant keep magnetic
frequency, field constant.
Commenly used method
 In order to b produced a high resolution NMR
spectrum of a sample there is need of
homogeneous magnetic field.
 The field strength might vary due to aging of the
magnet, movement of metal object near the
magnet, and temprature fluctuation.
 Types:-
1. external lock system
2. internal lock system
 By using this coils current is adjusted untill the
magnetic field has required homogeneity.
 Magnetic field produced by the shim coils cancel
the small residual inhomogeneities in the
magnetic field.
 These inhomogeneities could be caused by the
magnet design, material in the probe, variations
in the thickness of the sample tube, sample
permiability ,and ferromagnetic materials
arounds the magnet.
 A shim coil is designed to create a small magnetic
field, which will oppose and cancel out an
inhomogeneity in the B0 magnetic field.
 In which the sample holder is placed.
 Contains an air turbine to spin the sample holder,
while the spectrum is collect.
 Used to excite and detect the magnetization
inradio-frequency of sample.
 The most essential component is the RF
transmitting and receiving coil.
 For maximum sensitivity,a fixed frequency probe
is needed (mean a saparate probe is required for
each nucleus like 1H,13C,19F).
 4) Sweep Generator:
 To produce an amount of magnetic field pass
through the sample. For a nucleus to resonate, the
precession frequency should become equal to the
frequency of the applied RF radiation.
 This can be achieved by
 1) Frequency sweep method
 This method is used to resonate the nucleus.
 The frequency of the RF radiation is changed so that
it becomes equal to resonance frequency or
precession frequency
 2)Field sweep method
 In this method to resonate the nucleus the
frequency of the RF radiation is kept constant and
the precession frequency is changed by changing
the applied magnetic field.
 5) Radio Frequency Transmitter:
 The RF radiation is generated by RF crystal oscillator.
 The output of the oscillator is amplified, mixed and
filtered to produce monochromatic RF radiation and
delivered to the sample.
 A radio transmitter coil that produces short powerful
pulse of the radio waves.
 60 MHz capacity is normally used.
 6) RF receiver:
 A few turns wire is wound around the sample tube
tightly.
 The receiver coil is perpendicular to both the external
magnetic field and radio frequency oscillator.
 When RF radiation pass through the magnetized sample,
the resonance occurs, which cause the current voltage
across the coil to drop.
 7) Detector:
 when radiation is pass through the sample, the two
phenomena absorption and dispersion may occur.
 The observation of dispersion or absorption will
enable the resonance frequency to be determined.
 There are two method to detect the resonance
signals,
 A) single coil method ( radiofrequency bridge
method)
 B) double coil method ( nuclear induction method)
 A) single coil method(RF bridge) :
 In this method coil used for surrounding the
sample serves as both transmitter and receiver coil.
 The applied signals balanced against the received
signal and the resonance signal is recorded as an
out of balance e.m.f which may be amplified and
recorded.
 B) Double coil method (nuclear induction
method):
 In this method there are separate transmitter and
receiver coils.
 These two coils are fixed at right angle to each
other as well on the direction of external magnetic
field.
 This energy transfer is influenced by magnetic
nuclei in a sample placed between the two coils as
long as the RF current in the first coil was
resonance with nuclear transition.
 8)Amplifier & Recorder:
 The received signal is amplified by the help of
amplifier.
 And it is recorded by using a computer device.
 To avoid spectra dominated by the solvent signal,
most ‘H NMR spectra are recorded in a
deuterated solvent deuterium nucleus does not
respond, in the same region as the hydrogen
nucleus).
 However, deuteration is not “100%”, so signals
for the residual protons are observed. In
chloroform solvent (CDC1,). This corresponds to
CHCI, so a singlet signal is observed at 7.26 ppm.
 The following solvents are normally used in
which hydrogen replaced by deuterium.
 CS.
 CDCL.

 Carbon disulfide.
 Deuteriochloroform.
 CDCI, is a common solvent used for NMR
analysis. It is used because most compounds will
dissolve in it, it is volatile and therefore easy to
get rid of.
 Hexa deuteriobenzene
 NMR is used in biology to study the Biofluids,
Cells, Perfused organs and biomacromolecules such
as Nucleic acids(DNA, RNA), carbohydrates
Proteins and peptides. And also Labeling studies in
biochemistry.
 NMR is used in physics and physical chemistry to
study High pressure diffusion ,Liquid crystals
,liquid crystal solutions, Membranes, Rigid solids.
 NMR is used in food science.

 NMR is used in pharmaceutical science to study

Pharmaceuticals and Drug metabolism.
NMR is used in chemistry to :
 Determine the Enantiomeric purity.
 Elucidate Chemical structure of organic and
inorganic compounds.
 Macromolecules –ligand interaction.
 H-NMR APPLICATIONS
 H-NMR widely used for structure elucidation.
 Inorganic solids- In organic compounds are
investigated by solid state 1H-NMR.eg CaSO4.H20.
 Organic solids- Solid-state H-NMR constitutes a
powerful approach to investigate the hydrogen-
bonding and ionization states of small organic
compounds.
 Direct correlation with hydrogen-bonding lengths
could be demonstrated, e.g. for amino acid carboxyl
group.
 Polymers and rubbers- Examine hydrogen bonding
and acidity. Peptides and proteins.
 Clinical and scientific research.
In vivo NMR studies
 Concerned with ‘H NMR is spectroscopical
studies of human brain.
 Many studies are concerned with altered levels of
metabolites in various brain diseases.
 To determine the spatial distribution of any given
metabolite detected spectroscopically IS (image
selected in vivo spectroscopy).
 Reference:
 https://www.slideshare.net/himajadonthula/
nmr-spectroscopy-by-himaja-donthula
 https://www.slideshare.net/NaveenBalaji32/n
mr-instrumentation-naveen-balaji