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    C NMR Spectros

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    Ahmad AlShahrour
    13C NMR spectroscopy provides information about carbon atoms in a molecule. Despite carbon-13 having low natural abundance and sensitivity, modern techniques like signal averaging and higher magnetic fields allow its routine observation. Proton-decoupled 13C NMR yields a simple spectrum with one peak per chemically distinct carbon. Chemical shifts cover a wide range and provide information about hybridization and molecular structure. Different 13C NMR techniques like attached proton test and distortionless enhancement by polarization transfer distinguish carbon types based on their protonation.

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    C NMR Spectros

    Uploaded by

    Ahmad AlShahrour
    13 views17 pages
    13C NMR spectroscopy provides information about carbon atoms in a molecule. Despite carbon-13 having low natural abundance and sensitivity, modern techniques like signal averaging and higher magnetic fields allow its routine observation. Proton-decoupled 13C NMR yields a simple spectrum with one peak per chemically distinct carbon. Chemical shifts cover a wide range and provide information about hybridization and molecular structure. Different 13C NMR techniques like attached proton test and distortionless enhancement by polarization transfer distinguish carbon types based on their protonation.

    Original Description:

    Carbon­13

    Original Title

    Carbon­13

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    13C NMR spectroscopy provides information about carbon atoms in a molecule. Despite carbon-13 having low natural abundance and sensitivity, modern techniques like signal averaging and higher magnetic fields allow its routine observation. Proton-decoupled 13C NMR yields a simple spectrum with one peak per chemically distinct carbon. Chemical shifts cover a wide range and provide information about hybridization and molecular structure. Different 13C NMR techniques like attached proton test and distortionless enhancement by polarization transfer distinguish carbon types based on their protonation.

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    © All Rights Reserved
    Download as PPT, PDF, TXT or read online from Scribd
    Download as ppt, pdf, or txt
    13 views17 pages

    C NMR Spectros

    Uploaded by

    Ahmad AlShahrour
    13C NMR spectroscopy provides information about carbon atoms in a molecule. Despite carbon-13 having low natural abundance and sensitivity, modern techniques like signal averaging and higher magnetic fields allow its routine observation. Proton-decoupled 13C NMR yields a simple spectrum with one peak per chemically distinct carbon. Chemical shifts cover a wide range and provide information about hybridization and molecular structure. Different 13C NMR techniques like attached proton test and distortionless enhancement by polarization transfer distinguish carbon types based on their protonation.

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    © All Rights Reserved
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    of 17

    C NMR spectroscopy

    13

    -Despite the low natural abundance (only 1.1%)


    and relatively low sensitivity of the 13C nucleus,
    its observation is now made routine by the use
    of efficient signal averaging, made possible by
    the pulse-FT approach, and by the availability
    of higher magnetic field strengths. However,
    sample quantity requirements are still
    approximately ten times those for proton
    observation.
    -Due to low abundance of 13C there is no
    chance of finding two 13C nuclei in adjacent
    position within a molecule so that homonuclear
    13C-13C couplings are not observed.

    -The resulting carbon spectrum then has a


    surprisingly simple appearance; a single line is
    observed for each chemically distinct carbon in
    the molecule, in the absence of further
    coupling to nuclei other than protons.
    Chemical shifts and resonance intensities
    -The chemical shift range for the carbon-13
    nucleus is much greater than that of the proton,
    covering a typical range of 0-220 ppm, again
    with the shift of tetramethylsilane assigned as
    0.0 ppm.
    -The value of δ in 13C is 20 times greater than
    the value of δ eg protons.
    -For example, aromatic protons resonate at
    around 7 ppm whereas aromatic carbons are to
    be found around 140 ppm.
    -All factors affect the δ of protons are applied to
    carbon.
    Different techniques of 13C-NMR

    1. Undecoupled 13C-NMR
    - One of the most important problems in CMR
    measurements was the splitting of each carbon
    signal with the attached proton 1J (125-160 HZ

    and sometimes up to 250 HZ), the next carbon

    protons 2J, 3J (≈ 10-30 HZ).


    2. Proton decoupled 13C-NMR (decoupled
    13C-NMR)

    -The technique of double irradiation


    discussed before was applied. Thus,
    broadband irradiation in the proton region
    while recording the CMR decouples all
    protons from the obtained spectrum. Hence
    each type of carbons in the molecule will
    give only a singlet signal.
    -Thus the number of signals obtained indicate the
    number of different types of carbons present in the
    molecule.
    - Electronegativity, hybridization, and anisotropy
    effects all affects 13C chemical shifts just as
    they do for protons, but in a more complex
    fashion.
    - One of the most powerful features of 13C
    spectra is that they allow one to determine the
    number of different carbons in a molecule and
    thus allow a recognition of equivalences or
    symmetry elements. For instance,
    cyclooctatraene readily dimerizes to a solid. On
    the basis of theory, two possible structures can
    be proposed for tins dimer.
    -1,2– and 1,3– Dichlorobenzene provide
    another easy example of the utility of 13C
    spectra.
    -1,2–Dichoro–benzene has a plane of
    symmetry which gives it only three different
    types of carbon atoms. 1,3– Dichlorobenzene
    has a plane of symmetry which gives it four
    different types of carbon atoms.
    3. Off resonance proton decoupled 13C-
    NMR
    - One disadvantage of undecoupled CMR is
    the loss of information about the attached
    proton. For this reason another technique
    was introduced and this depend on-double
    irradiation also to avoid the coupling
    between the protons attached to adjacent
    carbon atoms.
    - This type of spectrum is known as Off Resonance
    Proton Decoupled 13C-NMR. In this spectrum
    each carbon split by its own protons. Thus, CH 3
    appears as quartet, CH2 as triplet, CH as doublet
    and C as singlet.
    * Example: eugenol
    4. Attached Proton Test (APT)
    - APT (Attached Proton Test CMR) technique
    gives the CMR spectra as signals in two phases,
    in one phase lies the signals of even protonated
    carbons (C, CH2) and in the other phase lies the
    signals of the odd protonated carbons (CH,
    CH3). One can readily identify the phase of the
    even protonated carbons by the presence in the
    same phase of signals due to the solvent.
    5. Destortionless Enhancement by
    Polarization Transfer (DEPT)

    - In
    this technique, the carbon atom
    which attached to proton(s) will
    only give singlet signal but one
    cannot obtain a signal(s) for
    unprotonated carbon.

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