Journal
ANALYTICA CHIMICA ACTA
Volume 1110, Issue -, Pages 131-140Publisher
ELSEVIER
DOI: 10.1016/j.aca.2020.03.014
Keywords
Pure shift NMR; Zangger-sterk; PSYCHE; TSE-PSYCHE; CSSF-TOCSY; Fischer-tropsch waste-water
Categories
Funding
- National Natural Science Foundation of China [U1710106]
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Fischer-Tropsch (F-T) process is an important synthesis route to acquire clean liquid fuels through modern coal chemical industry, which converts syngas (CO and H-2) into hydrocarbon, and also generates oxygenates discharged as the F-T waste-water. These oxygen-containing compounds in F-T waste-water have the similar molecular weight and some are even isomers of each other. Hence, it is necessary to develop rapid and efficient analysis tools to obtain identification and quantitative information of the F-T waste-water. The pure shift NMR techniques provided only chemical shift information in one-dimension H-1 NMR spectra, without homonuclear J(H-H) coupling. In this work, we tested and compared three pure shift NMR techniques (including Zangger-Sterk, PSYCHE and TSE-PSYCHE methods) in the analysis of two F-T waste-water model mixtures, genuine waste-water and two alcohol isomer mixtures. The results show that J(H-H) coupling multiplicities are collapsed into singlets corresponding to individual chemically distinct protons of the compound. For some severely overlapped signals in the pure shift NMR spectra, the chemical shift selective filters with TOCSY (CSSF-TOCSY) experiments were conducted to assist the signal assignment. Thus, pure shift NMR approaches can identify most signals of components, and CSSF-TOCSY can extract the signal of a specific compound. The combination of these two NMR techniques offers a powerful tool to analyze the F-T waste-water or other complex mixtures including isomer mixtures. (C) 2020 Elsevier B.V. All rights reserved.
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