Development of an HPLC, GC/MS method for analysis of HYGAS oil samples
Direct analysis of a HYGAS oil sample by gas chromatography/mass spectrometry (GC/MS) or capillary column GC/MS is difficult for at least two reasons: (1) due to the large number (probably over 400) of compounds present in the mixture, many overlapping peaks occur, resulting in mass spectra that are often confusing, and (2) moderately to highly polar compounds are not easily chromatographable. In Part 1 of this study, high performance liquid chromatographic (HPLC) methods for separating the complex HYGAS oil samples into fractions were investigated. A satisfactory separation of a HYGAS oil sample into seven fractions was achieved on a ..mu..Bondapak CN column with a complex gradient of hexane to THF. In Part 2, derivatization as a means for making polar compounds more amenable to identification by capillary column GC/MS was explored. With the use of standard phenols, carboxylic acids, amines, and alcohols, it was found that BSA (a silylating agent) was most effective in derivatizing phenols and alcohols and Methyl-8 Concentrate (an alkylating agent) was most effective in derivatizing carboxylic acids and amines. In Part 3, a preliminary study of the methods developed in Parts 1 and 2, namely HPLC separation into fractions and derivatization of the polar fractions, was undertaken on an authentic HYGAS oil sample to determine whether the methods would make the sample more amenable to analysis by capillary column GC/MS. It was found that, with HPLC, the complex mixtures of HYGAS oil samples are separated into simpler complex mixtures and, with derivatization of the polar fractions, the identification by capillary column GC/MS of polar compounds not normally chromatographable was enhanced.
- Research Organization:
- Argonne National Lab. (ANL), Argonne, IL (United States)
- Sponsoring Organization:
- USDOE
- DOE Contract Number:
- W-31-109-ENG-38
- OSTI ID:
- 5769895
- Report Number(s):
- ANL/EMR-4
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
COAL LIQUIDS
FRACTIONATION
GAS CHROMATOGRAPHY
LIQUID COLUMN CHROMATOGRAPHY
MASS SPECTROSCOPY
CHEMICAL REACTIONS
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HYGAS PROCESS
POLYCYCLIC AROMATIC HYDROCARBONS
QUALITATIVE CHEMICAL ANALYSIS
AROMATICS
CHEMICAL ANALYSIS
CHROMATOGRAPHY
GASIFICATION
HYDROCARBONS
ORGANIC COMPOUNDS
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THERMOCHEMICAL PROCESSES
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