Synthesis of oligomeric models of coal derived materials for use with GPC calibration. Quarterly report, January-March 1984

Technical Report · Sun Apr 01 04:00:00 EST 1984

OSTI ID:5000514

Baltisberger, R J; Jones, M B

The purpose of this study was to develop a set of GPC calibration standards for asphaltene and preasphaltene analysis. A series of oligo(arylether) (1) and oligo(arylmethylenes) (2) from 170 to 580 g/mole were prepared via modified Ullmann-type reactions (ethers) and condensation of an aryl lithium derivative with an aryl carboxaldehyde, followed by reduction of the resulting carbonol (methylenes). These compounds were examined as molecular weight calibration standards for GPC analysis. A nearly linear plot was found to exist between the logarithm of molecular weight times mol fraction hydrogen versus retention volume with THF as the solvent. Further this plot was coincident with commercial polystyrene standards (600 to 2000 g/mol) and with the majority of our lignite derived asphaltenes and preasphaltenes. Work in our laboratory suggests that universal calibration plots for the gel permeation chromatographic (GPC) analysis of lignite derived preasphaltene and asphaltene liquefaction products are possible for determining number and weighted average molecular weight values. The data indicates that the acid content (OH mmol/g) and the hydrogen content (mole fraction or H/C mole ratio) are representative of the solubility parameters of the asphaltenes/preasphaltenes. Universal calibration plots based on the logarithm of the hydrodynamic volume, number average molecular weight times hydrogen content, result in a smooth curve coincident with polystyrene standards, model compounds, and lignite derived asphaltenes/preasphaltenes. The data supports an hypothesis that two factors, degree of condensation of the aromatic carbons and acetate content, determine the size-molecular weight relationships of the coal derived molecules. 19 references, 5 tables, 9 figures.

• Research Organization: North Dakota Univ., Grand Forks (USA)
• DOE Contract Number: FG22-81PC40810
• OSTI ID: 5000514
• Report Number(s): DOE/PC/40810-9; ON: DE84011520
• Country of Publication: United States
• Language: English

Related Subjects

01 COAL, LIGNITE, AND PEAT
010405* -- Coal
Lignite
& Peat-- Hydrogenation & Liquefaction
ASPHALTENES
ASPHALTS
BITUMENS
CALIBRATION
CHROMATOGRAPHY
COAL LIQUIDS
FLUIDS
GEL PERMEATION CHROMATOGRAPHY
LIQUIDS
MOLECULAR WEIGHT
ORGANIC COMPOUNDS
OTHER ORGANIC COMPOUNDS
SEPARATION PROCESSES
STRUCTURAL MODELS
SYNTHESIS
TAR