Sensitivity-enhanced quantitative 13C NMR spectroscopy via cancellation of 1J(CH) dependence in DEPT polarization transfers.
A scheme has been developed to eliminate virtually all signal intensity dependence on 1JCH in polarization transfers between 1H and 13C nuclei, reducing differences in signal intensity to only 1.5% over the entire natural 1JCH range. The scheme relies on the summation of time-domain data acquired with four suitably selected Delta delays so that the J dependence is essentially canceled in the final, signal-averaged free-induction decay. These Delta delays have been incorporated into the DEPT pulse sequence to create sensitivity-enhanced experiments for collecting quantitative 13C{1H} spectra. Four experiments, each with unique read pulse angles, give quantitative spectra with 200-300% more sensitivity than conventional 13C spectra acquired with inverse-gated 1H decoupling. The experiments are ideal for recording spectra with improved quantitative information or for substantially reducing the long acquisition times indicative of quantitative 13C experiments. The ability of the experiments to provide quantitative spectra was demonstrated with a simple ethylbenzene solution, however, they can easily be adapted to various applications for analysis of complex mixtures.
Henderson
Terry J
TJ
U.S. Army Edgewood Chemical Biological Forensic Analytical Center, AMSRD-ECB-RT-AF, E5100, 5183 Black Hawk Road, Aberdeen Proving Ground, Maryland 21010-5424, USA. txhender@apgea.army.mil