Abstract

The direct on-line coupling of supercritical fluid chromatography and proton high-field nuclear magnetic resonance spectroscopy is demonstrated. For this purpose, a specially designed pressure-proof continuous-flow probe head has been developed, from which a signal line width of 1.5 Hz can be obtained in the supercritical state. A separation of phthalates is carried out under supercritical conditions with carbon dioxide as eluent and is monitored on-line with 1 H NMR on a 400-MHz NMR instrument. All the components can be identified from their NMR spectra. The advantage of carbon dioxide as eluent is that the whole spectral range of the 1 H NMR spectra can be observed and no solvent suppression techniques are necessary to obtain the NMR spectra

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