Blood, sweat, and tears. Toward a rehabilitation of the INADEQUATE experiment

The double-quantum-filtered carbon-carbon correlation experiment (INADEQUATE) can be accelerated significantly through a reduction in the spin-lattice relaxation times by dissolving oxygen gas in the solution. The effect is enhanced by lowering the temperature and by pressurizing the sample tube with oxygen. This offers a fourfold reduction in the relaxation times of the carbon-13 resonances in the 125-MHz spectrum of methyl salicylate. The addition of perfluorotertiarybutanol (related to the artificial blood substitutes) increases the amount of oxygen that can be dissolved, so that without oxygen pressurization, similar reductions in the relaxation times can be achieved. The nuclear Overhauser enhancements are only slightly reduced by addition of oxygen. Polarization transfer from the directly attached protons (INEPT) further increases the sensitivity if at least one of the two coupled carbon sites is protonated, principally because the proton spin-lattice relaxation times of oxygenated samples are shortened by the relaxation agent. These modest improvements in sensitivity are in general complementary to existing enhancement schemes. (C) 1998 Academic Press.