Development and evaluation of supercritical fluid chromatography/mass spectrometry for polar and high molecular weight coal components

Conference · Mon Sep 01 04:00:00 EDT 1986

OSTI ID:5165351

Chess, E K; Smith, R D

Supercritical fluid chromatography offers the capability of separating nonvolatile and thermally labile compounds impossible to separate by gas chromatography (GC) and the introduction of nonvolatile or thermally labile compounds for mass spectrometric and analysis is an important area of research in MS. However, current methods, such as field desorption (FD), desorption chemical ionization (DCI), laser desorption (LD), and a suite of particle bombardment techniques, such as secondary ion mass spectrometry (SIMS) fast atom bombardment (FAB), and /sup 252/Cf-plasma desorption mass spectrometry (/sup 252/Cf-PDMS), are subject to difficulties. These include: matrix effects, complex mass spectra, responses which vary greatly with compound polarity, difficult quantitation, spectra which are difficult to predict and interpret, and sensitivity to the nature of the substrate support surfaces. The development of the DFI interface in our laboratory has resulted in establishing methods for the direct characterization of supercritical fluids and has demonstrated the feasibility of the combined capillary column SFC/MS. This approach allows relatively high molecular weight compounds to be efficiently separated and analyzed, with detection limits generally in the picogram range. Our work has shown that excellent ''soft'' chemical ionization (CI) spectra, amenable to quantitation, can be obtained for any compound soluble in a supercritical fluid. 8 refs., 3 figs.

• Research Organization: Pacific Northwest Lab., Richland, WA (USA)
• DOE Contract Number: AC06-76RL01830
• OSTI ID: 5165351
• Report Number(s): PNL-SA-14231; CONF-860961-3; ON: DE87000820
• Country of Publication: United States
• Language: English

Related Subjects

01 COAL, LIGNITE, AND PEAT
010600* -- Coal
Lignite
& Peat-- Properties & Composition
CHROMATOGRAPHY
COAL LIQUIDS
FLUIDS
LIQUIDS
MASS SPECTROSCOPY
SEPARATION PROCESSES
SPECTROSCOPY
SUPERCRITICAL FLUID CHROMATOGRAPHY