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Title: Simulated distillation of high-boiling petroleum fractions by capillary supercritical fluid chromatography and vacuum thermal gravimetric analysis

Journal Article · · Anal. Chem.; (United States)
DOI:https://doi.org/10.1021/ac00137a005· OSTI ID:6569497

Capillary supercritical fluid chromatography (SFC) and vacuum thermal gravimetric analysis (VTGA) were utilized for simulated distillation (SIMDIS) of high-boiling petroleum fractions obtained by short-path vacuum distillation. The SFC method covers the approximate boiling range of 250-1400/sup 0/F. Under the present conditions, even 42% of a nondistillable, nondeasphalted residue was recovered from the column at a calculated 1426/sup 0/F atmospheric equivalent boiling point. The influence of temperature and pressure on resolution and retention was studied. SFC-SIMDIS was performed by using linear pressure programming at 100/sup 0/C, as compared to 400/sup 0/C+ temperatures required for comparable samples when capillary gas chromatography (GC) is employed. Polysiloxane-coated, 50-..mu..m-i.d. columns permitted fast analyses (30-min run time) yet maintained adequate resolution for SIMDIS analysis. VTGA-SIMDIS data of samples in the 500-1000/sup 0/F boiling range yielded excellent correlation with actual distillation data. However, thermal analysis revealed decomposition of samples at temperatures exceeding ca. 370/sup 0/C. The validity of the SFC method was demonstrated by comparing SFC-SIMDIS data with those obtained by GC and VTGA.

Research Organization:
Brownlee Labs., Santa Clara, CA
OSTI ID:
6569497
Journal Information:
Anal. Chem.; (United States), Vol. 59:10
Country of Publication:
United States
Language:
English