Mass spectrometric analytical services and research. Annual progress report and quarterly report for the period December 9, 1975--March 8, 1976 activities to support coal-liquid characterization research

Technical Report · Thu Mar 25 04:00:00 EST 1976

DOI:https://doi.org/10.2172/7196449· OSTI ID:7196449

Scheppele, S E

Interfacing of a Perkin Elmer model 3920 gas chromatograph to the CEC 21-110B mass spectrometer has been completed and the GC/MS system is operational. Detailed descriptions of the heated probe assembly and the rapid mass-scanning module are given. Initial emphasis has been placed on the utilization of GC/MS in conjunction with field ionization (FI). Satisfactory results have been obtained. The FI source for the CEC 21-110B mass spectrometer is routinely operational. Familiarity with its operation has improved ion-abundance reproducibility. For a mixture containing aromatic hydrocarbons, thiophenes, and furans, the average percent standard deviation in the average percent ionizations is 3.55 percent from three spectra. Application of the technique of FI mass spectrometry to quantitative analysis of coal type mixtures has been explored. The consequences of sensitivity data on the analytical results have been considered. Relative weight and mole sensitivities have been determined for 30 aromatic hydrocarbons, 20 thiophenes, and 7 heteroatom (oxygen and nitrogen) containing compounds with respect to ethylbenzene. Excellent analytical data has been obtained from three known mixtures using these sensitivities. Fifty three coal-liquid samples have been processed. Empirical formulas for 5000 ions have been determined from the high-resolution (70 eV) spectra recorded on photographic plates. FI spectra have been recorded for 20 synthoil samples. Percent ionizations obtained from these spectra have been used to characterize the mixtures according to Z numbers. (auth)

• Research Organization: Oklahoma State Univ., Stillwater (USA). Dept. of Chemistry
• Sponsoring Organization: US Energy Research and Development Administration (ERDA)
• OSTI ID: 7196449
• Report Number(s): BERC-0020-3
• Country of Publication: United States
• Language: English

Related Subjects

01 COAL, LIGNITE, AND PEAT
010600* -- Coal
Lignite
& Peat-- Properties & Composition
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400100 -- Analytical & Separations Chemistry
CHEMICAL COMPOSITION
CHROMATOGRAPHY
COAL LIQUEFACTION
COAL LIQUIDS
FUELS
GAS CHROMATOGRAPHY
LIQUEFACTION
MASS SPECTROMETERS
MEASURING INSTRUMENTS
RESEARCH PROGRAMS
SEPARATION PROCESSES
SPECTROMETERS
SYNTHETIC FUELS