TUTORIAL CHM580

CHAPTER 9 – NMR spectroscopy

1. What do you understand from the term NMR spectroscopy.

a) Describe the most common type of magnet used with high resolution NMR
spectrometers.
b) What is the advantage of this magnet?
c) What is the effect of increasing the magnetic field strength in NMR?

2. In NMR spectroscopy what are the advantages of using a magnet with high magnetic
field.

Ans: The sensitivity improves with field strength

3. Briefly explain the use of the following features in proton NMR spectrum
a) Number of signal - provides information about the number of types of different (or
equivalent) protons in a compound
b) Chemical shift - provides information about the electronic environment of the protons
in a compound
c) Integral - provides information about the number of protons for that particular signal
d) Peak multiplicity - provides information about the number of neighbouring protons of
each protons in the compound

4. What type of solvents is used in NMR? Explain why.

Ans: Deuterated solvent. Why?

5. Define the chemical shift, δ. Describe two factors that affect the proton chemical shift
values.

Ans: Electronegativity of nearby atoms and hybridization. Elaborate.

6. Explain how an NMR spectrum is obtained in Fourier transform-nuclear magnetic

resonance (FT-NMR) spectrometer

Ans:

Sample nuclei have magnetic dipole moment. The dipole moment is under influences of
external magnetic field, Bo. Some are parallel and antiparallel to the field.

Once equilibrium has reached, the dipoles that parallel to external magnetic field is little
bit greater in population. This will results a net magnetization, Mz and behave as a
magnet. An electrical current applied to a coil of wire surrounding a magnet (Mz) will
cause the magnet to rotate.

An RF pulse through a coil of wire around the sample is used to generate a second
magnetic field, B1 at 900 to Bo. This provides the excitation process in NMR. B1 is applied
as a pulse for a very short of time.

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The net magnetic moment of sample is shifted out of alignment with Bo by the pulse of
B1. When the pulse is discontinued, the excited nuclei precess around the applied
magnetic field at an angle of B o. This ‘rotating magnet’ induces current in the wire coil.
This induced current is the NMR signal.

The signal undergoes free induction decay (FID). The current decreases with time as
the freely precessing nuclei back to ground state. The FID signal is time-domain signal
and must be processed using the FT to produce frequency domain spectrum.

7. Give two reasons why tetramethylsilane (TMS), (CH3)4Si is used as standard reference
in 1H and some 13C NMR analyses.

Ans: 1) Because all the protons are identical and

2) Absorbed at an unusually high field strength, large amount of electron shielding in
TMS (caused by electropositive silicon), therefore it signal appear at nearly 0 ppm
chemical shift and is used as standard reference.

8. Explain why is 13C - 13C spin-spin splitting not observed in typical organic compounds.

Ans: The natural abundance of 13C is very low, less than one 13C per molecule. The
probability of finding two adjacent 13Cs is very low, therefore there is no 13C-13C splitting.
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9. C NMR is usually decoupled. Briefly explain how decoupling is achieved.

Ans: In a hydrogen-decoupled mode, a samples is irradiated with two different RF: one to
excite all 13C nuclei and second is a broad spectrum of frequencies that causes all
hydrogens in the molecule to undergo rapid transitions between their nuclear spin states
(state saturation). On the time scale of a 13C-NMR spectrum, each hydrogen is in an
average constant nuclear spin state, with the result that 1H-13C spin-spin interactions are
not observed; they are decoupled

10. What is meant by ‘chemical equivalence’?

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