NMR (Nuclear Magnetic Resonance) Spectros

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NMR (Nuclear Magnetic Resonance)  1952: Nobel Prize in Physics to Purcell and Bloch

 1957: P. C. Lauterbur and Holm independently


Spectroscopy record 13C spectra
 1991: Nobel Prize in Chemistry to R. R. Ernst for
FT and 2D NMR
 2003: Nobel Prize in Medicine to P. C. Lauterbur and
P. Mansfield for MRI

The NMR Spectrometer

 NMR is an experiment in which the resonance


frequencies of nuclear magnetic spin systems are
investigated.
 NMR always employs some form of magnetic field
(usually a strong externally applied field B0)
 NMR is a form of both absorption and emission
spectroscopy, in which resonant radiation is
absorbed by an ensemble of nuclei in a sample,

The Use of NMR Spectroscopy


 Used to determine relative location of atoms within a
molecule
 Most helpful spectroscopic technique in organic
chemistry
 Maps carbon-hydrogen framework of molecules
 Depends on very strong magnetic fields

Things that can be learned in NMR Data


 Covalent chemical structure (“2D structure”)
– Which atoms/functional groups are present in a
molecule
– How the atoms are connected (covalently NMR Tube
bonded)
 3D Structure
– Conformation
– Stereochemistry
 Molecular motion
 Chemical dynamics and exchange
 Plus many more things of interest to chemists…

History of NMR
 1920-1930: physics begins to grasp the concepts of
electron and nuclear spin
 1936: C. J. Gorter (Netherlands) attempts to study 1H
and 7Li NMR with a resonance method, but fails
because of relaxation
 1945-1946: E. M. Purcell (Harvard) and F. Bloch
(Stanford) observe 1H NMR in 1 kg of paraffin at 30
MHz and in water at 8 MHz, respectively
Schematic Diagram of NMR Spectrometer

Instrumentation of NMR Spectrometer

Auto sampler

1. Sample Holder
- 5 mm glass tube is used, which can hold 0.4 ml liquid
- microtubes are used for low volume
2. Magnet
- the heart of NMR (accuracy and quality of the instrument
is
dependent on its strength)
Resolution increases with increase in the applied field
strength
Three types of magnets can be used
 Conventional Magnet (30 -60 MHz)
Evolution of NMR Instrument  Permanent or electromagnet ( 60 ,90, 100 MHz)
 Super conducting solenoids (high resolution)
Relationship between Bo and frequency (Larmor Frequency
equation)

Magnetic field Frequency

3.) Sweep generator – a set of Helmholtz coil located parallel


to the magnet, which alters the magnetic field
4.) RF transmitter – it is a pair of coils mounted perpendicular
to the path of field and receiver coil
5.) Receiver Coils and amplifier – amplifies the received EMR
by 105 times
6.) Detector- detected signal produced by the resonant nuclei.

Solvents

 Characteristics of Solvents
- chemically inert solvent is used
- solvents should be magnetically isotopic in
nature (2H = Deuterium)
- free from any hydrogen (1H)
- solvent should be able to dissolve the sample
in a reasonable quantity (approximately
10 % or more)

 Commonly used solvents


1. carbon tetrachloride (CCl4)
2. carbon disulfide (CS2)
3. deuterochloroform (CDCl3)
4. hexa Chloroacetone (CCl2)3CO
5. deuterodimethylsulfoxide ( CD3)2SO
6. deuterobenzene (C6D6)

NMR Principle

1. A nucleus can behave like a


magnet (because of its charge
and spin)
- Spin properties of Nuclei
- Spin has a quantum
property
 Nuclear spin is related to the
nucleon composition in a
nucleus

Nuclear Spin and Net Spin


I = ½ spherical charge distribution
I =3/2 – non –spherical charge distribution (electrical
quadropole magner ( exhibits electrical quadropolar
resonance)

Calculation of Spin State (I)


Quantum Description of NMR 2. NMR spectroscopy operates by applying a magnetic field to
nuclei and then measuring the amount of energy necessary to
 Nuclei of certain isotopes of elements have nuclear put various nuclei in resonance
spins because they are made up of protons and
neutrons, each of which has spin angular Alignment and Precession
momentum of h/4π.
Effect of external magnetic field in a spinning proton
 For a nucleus, the total spin angular momentum is
represented by It, the spin quantum number by I and
the z component of nuclear spin by Iz .
 /I/ = [I(I+1)]1/2 h/4π and Iz = mh/4π
 ml = -l, -l +1, -l +2,
 ml = 2l +1
 Example: A proton has spin ½, in the presence of
magnetic field, it has two states, a state of lower
energy field ( aligned to the field, m l = +1/2) and a
state of higher energy (opposed to the field, ml -1/2)
 Nitrogen(14 N), I =1, has three possible orientations in
a magnetic field because I =1, ml = -1,0,1

Other Properties of Atomic Nuclei

 Nuclei with spin > ½ have a quadrupolar moment and


are capable of coupling with electric field gradients

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