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C-13 NMR

Carbon-13 NMR requires higher numbers of scans than proton NMR due to the low natural abundance and magnetogyric ratio of carbon-13. Electronegativity, hybridization, and anisotropy affect carbon-13 chemical shifts in a similar way to proton shifts but are about 20 times larger. Carbon-13 spectra show one peak for each non-equivalent carbon, and coupling between neighboring carbon-13 nuclei is not observed due to low probability of two adjacent carbon-13s. DEPT experiments distinguish between carbon types based on the number of directly bonded hydrogens.

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30 views

C-13 NMR

Carbon-13 NMR requires higher numbers of scans than proton NMR due to the low natural abundance and magnetogyric ratio of carbon-13. Electronegativity, hybridization, and anisotropy affect carbon-13 chemical shifts in a similar way to proton shifts but are about 20 times larger. Carbon-13 spectra show one peak for each non-equivalent carbon, and coupling between neighboring carbon-13 nuclei is not observed due to low probability of two adjacent carbon-13s. DEPT experiments distinguish between carbon types based on the number of directly bonded hydrogens.

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EnesEmreTaş
Copyright
© © All Rights Reserved
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Download as PPTX, PDF, TXT or read online on Scribd
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Carbon-13 NMR

13Cnuclei have spin, act like magnets and interact with the outside magnetic field
Natural abundance of carbon-13 is very low (1.08%) and its magnetogyric ratio is
smaller than that of H, so higher number of NMR scans are required.
! Remember as dE increases so does the excess population
and the NMR signal
Electronegativity,
hybridization and
anisotropy affect 13C
shifts same fashion as
H but about 20 times
larger. H is one bond
further away from the
shielding/deshielding
factors.
Anisotropy in action

One peak for each non-equivalent carbon-13


An unexpected small upfield shift caused by Oxygen

Reliable NMR signals allow for predictive calculations of carbon-13 shifts, above predictions
are 0.1 ppm away from experimental results
PROTON COUPLING AND SPIN-SPIN SPLITTING IN 13C SPECTRA
(Two neighboring 13C is very low probability, so no 13C- 13C coupling observed)

Typical 13C coupling constant values are between 100-250 Hz


SATURATION
If too high radio frequency (rf) is applied, the
excited nuclei may not return to the ground state
in time. This will eliminate the slight excess in
the ground state and very soon both energy
levels become equally populated. At this
condition, there will be no net absorption of (rf)
and the peak intensity will diminish to zero.
Therefore it is very important to adjust (rf)
power level properly.
Peak intensities are enhanced due to
Nuclear Overhauser Effect
Nuclear Overhauser Effect:

*NOE result in different extents of peak enhancement for –CH-,


-CH2-, -CH3

*NOE and long (out of range) relaxations for some types of


carbons prevent reliable integration values for carbon-13 spectra
CH3-CH2 –CH2 –OH
In off-resonance coupling,
Low level of coupling is retained,
revealing the effects of directly attached
protons and also lowering coupling constants
“DEPT” EXPERIMENT
(Distortionless Enhancement by Polarization Transfer)
In this experiment a complex series of pulses
are applied on the sample. These pulse
sequences causes different interactions
between the 13C and the hydrogen atoms
directly bonded to it. As a result the signals
obtained will be either positive or negative
depending on the number of hydrogen atoms
on the carbon atom.
-CH2- peaks appear as negative resonances

Only carbons with single hydrogen

Subspectra of DEPT
experiment for
isopentyl acetate
Only protonated carbons
Examples of Carbon-13 Spectra:
Equivalent Carbons
Aromatics:
CD3-SO-CD3
A septet that
does not obey the
Pascal Triangle,
but a different
distribution of
spin possibilities
e.g. CDCl3

CDCl3

e.g. Acetone-d5
Rapid quadrupolar relaxation of Cl, Br and I nuclei is the
reason we don't normally see any indication of coupling
between these nuclei and adjacent carbons or protons

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