SEMINAR ON 13 CNMR SPLITTING AND DECOUPLING METHODS

Contents : Introduction 13 CMR Splitting Decoupling Methods Noise Decoupling Off Resonance Decoupling Selective Proton Decoupling Nuclear Overhouser Effect References

INTRODUCTION :
12C isotope of C => I=0, magnetically inactive 13C => I = 1/2, 1H => I = In 13CNMR, following important information can be obtained => Gives direct information about the Carbon Skeleton. No. of equivalent carbons. No. of hydrogens attached. Tells about the hybridization of carbon. To identify Carbonyl Carbon.

In a 1.9 T field, the precision frequency of 13C is 20 MHz. For 1H => 80 MHz. 12C being non-magnetic. 13 CMR-Splitting : The interaction of the spin of nucleus with that of spin of other nucleus adjacent to it results in splitting. Ex CH2

SPIN-DECOUPLING STUDIES :

METHODS

IN

13

CNMR

1. Noise Decoupling : => by double irradiation of 1H at their resonance frequency. i.e. at 80 MHz 1.9 T. => all protons are simultaneously double irradiated. Ex : Spectrum

2.

Off Resonance Decoupling : => Sample is irradiated at a frequency close to (but not identical at resonance frequency of protons). => does not remove in residual coupling while long range coupling is usually lost. Methines H C Methylene H C Methyl H C

Quarternary Carbons

3.

H H (doublet) (triplet) (quatret) Selective Proton Resonance Decoupling :

Nuclear Overhauser Effect : Used to demonstrate that two nuclei are in close proximity within the molecule. to identify Carbonyl Carbon. Ex : Consider a hypothetical molecule Ha Hb C C

 If we double irradiate H6, then, relaxation of Ha will be speeded up, thus decreases relaxation time. E t = Constant Thus E will increase, i.e. increase in the intensity of MMR signal of Ha.

REFERENCES :
Organic Spectroscopy by William Kemp, Palgrave 3rd Edition, P.No.177-193. A textbook of Organic Spectroscopy by Silverstain, P.No. 217-249. Instrumental methods of chemical analysis by B.K. Sharma. P.No. 554-570. Elementary Organic Spectroscopy by V.R. Sharma P.No.137, 198.