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Title: Heteroatom speciation in coal liquefaction via FT-IR coupled with liquid chromatography. Quarterly progress report, January 1, 1983-March 31, 1983

Technical Report ·
OSTI ID:6044301

Flow cell Fourier Transform Infrared (FTIR) spectrometric detection of a wide variety of compounds separated by high performance liquid chromatography (HPLC) has become a useful tool in our laboratory for the elucidation of component structure in complex mixture analyses. HPLC/FTIR has, until recently, been accomplished only with semi-preparative or analytical-scale chromatography. By virtue of the relatively large volumes of elution solvent that are necessary on these scales, many infrared window-rich or exotic solvents have been too expensive to use routinely. Coupling of microbore HPLC columns to the FTIR has been shown to directly address this problem, and qualitatively the detectability appears comparable to the other chromatographic scales. The encouraging qualitative results from the semi-preparative/analytical/microbore HPLC/FTIR study which we have previously reported has prompted the following work on quantitation. For this study the primary effort was directed toward how increasing retention affects the detection limits of a particular type of compound. A series of nonpolar compound was chosen because of their known separation characteristics on silica gel. It was found that the signal to noise ratio decreases with increasing retention, probably due to the fixed sampling rate of the FTIR software used, but possibly also for other reasons considered. Detection limits were determined for toluene and other compounds.

Research Organization:
Virginia Polytechnic Inst. and State Univ., Blacksburg (USA)
DOE Contract Number:
FG22-81PC40799
OSTI ID:
6044301
Report Number(s):
DOE/PC/40799-T6; ON: DE83011910
Country of Publication:
United States
Language:
English