Aa. Herod et al., COMPARISON OF FAST-ATOM-BOMBARDMENT MASS-SPECTROMETRY AND SIZE-EXCLUSION CHROMATOGRAPHY IN DEFINING HIGH-MOLECULAR MASSES IN COAL-DERIVED MATERIALS, Fuel, 72(9), 1993, pp. 1317-1325
The detection by fast atom bombardment mass spectrometry (f.a.b.-m.s.)
of high molecular mass (greater than 1000 Da) material in coal-derive
d products was investigated. The pentane insoluble (PI) fractions of l
iquefaction extracts from maceral concentrates of two UK coals (Linby
and Cortonwood), prepared in a low-residence time (less than 10s) flow
ing-solvent reactor and fractions of hydropyrolysis tar prepared in a
hot-rod reactor at 500-degrees-C were examined. F.a.b.-m.s. spectra of
the Cortonwood liptinite concentrate liquefaction extract PI-fraction
mounted in a thiodiethanol matrix indicated ions up to molecular mass
es of about 4000 Da. This appears to be the highest reported molecular
mass identified by fast atom bombardment in a coal-derived material.
Other liquefaction extract PI-fractions showed somewhat lower molecula
r masses. The phenolic, basic nitrogen and aromatic fractions of the h
ydropyrolysis tar indicated ionization up to molecular mass limits bet
ween 1500 and 2000 Da. Comparison of these results with size exclusion
chromatography (s.e.c.) showed agreement with results for the hydropy
rolysis tar fractions; however, the presence of molecular masses in ex
cess of 10 000 Da was indicated by s.e.c. for the liquefaction extract
PI-fractions. Not all problems associated with vaporization, ionizati
on and detection of high molecular mass materials in f.a.b.-m.s. appea
r to have been solved, with the choice (polarity) and preparation of m
atrices for sample mounting remaining an empirical procedure.