Title page for ETD etd-08282003-155243
|Type of Document
||Amateis, Patricia Graham
||Feasibility of analysis of polar compounds by high performance liquid chromatography with Fourier transform infrared spectroscopic detection
|Taylor, Larry T.
|Bell, Harold M.
|Dorn, Harry C.
|Kingston, David G. I.
|McNair, Harold M.
- Liquid chromatography
- Fourier transform spectroscopy
|Date of Defense
High performance liquid chromatographic separations employing
on-line flow cell Fourier transform infrared spectroscopic
detection were developed for polar compounds including
phenols, alcohols, amines and azaarenes. Detection
by FTIR gave information concerning hydrogen bonding and
solvent effects occurring during the separations in addition
to giving structural information about eluted species to aid
in identification. Both analytical size and microbore normal
phase columns were employed. Such experimental considerations
as column overload, injected minimum detectable
quantities, the use of analytical vs. microbore columns and
flow cell pathlength were examined. The developed HPLC-FTIR
systems were applied to the analysis of several coal liquefaction
samples for heteroatom content. Confirmatory and
additional information concerning the samples were provided
by field ionization mass spectrometry, gas chromatography/
mass spectrometry and reversed phase liquid chromatography
employing UV detection. An equation relating reversed phase
retention times to structural parameters was developed and
applied to the analysis of the coal-derived samples. Two
process solvents were found to contain primarily alkyl-substituted phenols in addition to azaarenes such as pyridine
and quinoline. Some non-distillable coal-derived samples
were found to contain azaarenes such as alkyl quinolines.
Evidence was also found concerning the presence of hydroxypyridine
type compounds and the incorporation of process
solvent molecules into the coal structure during liquefaction.
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