Measurement of high-molecular-weight polycyclic aromatic hydrocarbons in soils by particle beam high-performance liquid chromatography-mass spectrometry.

Polycyclic aromatic hydrocarbons (PAHs) comprise a class of potentially hazardous com- pounds of concern to the U.S. EPA. The application of particle-beam (PB) liquid chromatography-mass spectrometry (LC-MS) to the measurement of high-molecular-weight PAHs was investigated. Instrument performance was evaluated for 16 PAHs in the molecular weight range 300-450 u. The PAHs were separated by reverse-phase high-performance liquid chromatography via a polymeric octadecylsilica (C-18) packing and gradient elution with methanol-tetrahydrofuran. On-column instrument detection limits, as measured by selected ion monitoring on the singly charged molecular ion of each PAH, were found to be 0.15-0.60 ng for PAHs with molecular weights up to 352 u and 2-4 ng for PAHs with molecular weights greater than 352 u. Instrument response was generally linear for PAHs with molecular weights 300-352 u and generally nonlinear for PAHs with molecular weights greater than 352 u. The PB electron impact mass spectra of the PAHs were found to vary with the ion distribution ratio of the singly charged molecular ion to the doubly charged molecular ion, dependent on molecular weight, ion source temperature, and concentration. Analysis by PB LC-MS was applied to extracts of PAH-spiked soil and a PAH-contaminated soil from the Pacific Northwest. Target analyte concentrations in the PAH-contaminated soil ranged from 0.85 to 84 µg/g. Quantitative estimates for nontarget PAHs also were determined. Analysis of a second soil extract from a hazardous waste site in the northeast part of the United States displayed isomeric patterns of high-molecular-weight PAHs similar to those of the Pacific Northwest extract.