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Separation and characterization of compound classes in coal liquids with chromatographic and spectral techniques

Thesis/Dissertation ·
OSTI ID:6313439
A variety of high-performance stationary phases were investigated with an array of mobile phases to determine which particular high-performance liquid chromatography (HPLC) systems could effect an efficient compound-class separation of polycyclic aromatic hydrocarbons (PAH), nitrogen heterocycles, and hydroxyl aromatics. The silica and Nucleosil NO2 HPLC systems, were investigated using the Snyder chromatographic adsorption model. After the chromatographic study of model compounds was completed, PAH, nitrogen heterocycle, and hydroxyl aromatic fractions were isolated from a Wyodak solvent refined coal sample using a Chromosorb-T/basic alumina procedure. The nitrogen heterocycle and hydroxyl aromatic open-column fractions were further separated using a silica normal-phase HPLC system. The HPLC system incorporating a DMSO:carbon tetrachloride mobile phase and a silica stationary phase further separated the nitrogen compound and hydroxyl aromatic Chromosorb-T/basic alumina open-column fractions. In addition, a chromatographic backflush method was developed to isolate polyfunctional compounds from nitrogen compound and hydroxyl aromatic open-column fractions. The HPLC subfractions were all characterized by infrared, nuclear magnetic resonance, and field ionization mass spectrometry (FIMS). The combined use of HPCL and FIMS was shown to be a powerful tool in the separation and characterization of very complex mixtures of PAH, nitrogen heterocycles, and hydroxyl aromatics in solvent refined coal liquids.
Research Organization:
Wyoming Univ., Laramie (USA)
OSTI ID:
6313439
Country of Publication:
United States
Language:
English