Determination of semivolatile and particulate polycyclic aromatic hydrocarbons in srm 1649a and PM2.5 samples by HPLC-fluorescence

The concentrations of 15 "priority pollutant" semivolatile and particulate polycyclic aromatic hydrocarbons (PAHs) were determined in three sets of samples supplied by the National Institute for Standards and Technology (NIST) as part of an interlaboratory analytical exercise. The put-pose of the exercise, organized by NIST and the U.S. Environmental Protection Agency, was to determine the comparability of measurements for various organic analytes among the participating laboratories, and to establish consensus values for SRM 1649a and interim materials. The commercially available SRM 1649a Atmospheric Urban Dust and two subsamples of this popular reference material were analyzed: an extract designated as Air Particulate Extract, and a resieved portion labeled Air Particulate I. The method used in our laboratory for the exercise consists of the extraction of the PAHs from the solid samples by ultrasonication, followed by separation and quantification using high-pet formance liquid chromatography-fluorescence detection. The accuracy and precision of the results obtained by our analytical protocol and by 14 other participating laboratories were evaluated using the International Union of Pure and Applied Chemistry, guidelines of z-scores (sigma = 25% of the exercise assigned value) and p-scores. Using these guidelines the accuracy of our method provided results that are satisfactory for all 15 target PAHs (\z\ less than or equal to 2) determined in the Air Particulate Extract and, except for fluorene, in the Air Particulate I sample. Finally, application of the methodology is demonstrated for the quantification of PAHs present at the pg (.) m(-3) range in PM2.5 samples collected from 163 m(3) of air in the Los Angeles basin.