title: Sampling and analysis of particulate matter by glow discharge atomic emission and mass spectrometries.
abstract: The direct introduction of particulate matter into glow discharge atomic emission and mass spectrometry sources through a particle beam/momentum separator apparatus is described. Vacuum action through a narrow (0.0625 in. i.d.) stainless steel tube allows the introduction of discrete samples of NIST SRM 1648 urban particulate matter (UPM) and caffeine in powder form. Introduction of "ambient" airborne particulate matter is also possible. Particles passing through the aerodynamic momentum separator impinge on the heated (∼200-250 °C) inner surface of the glow discharge plasma volume and are flash-vaporized. The resultant atoms/molecules are subjected to excitation/ionization collisions within the low-pressure (0.5-5 Torr of He or Ar) plasma, producing characteristic photon emission and/or signature ionic species. In this way, atomic emission and mass spectrometry identification of particle constituents is possible. Basic design aspects of the apparatus are presented, and demonstrations of atomic emission detection of the constituents in the NIST SRM illustrate the general characteristics of the approach. Transient atomic emission signals are captured for the introduction of preweighed, discrete samples, with the integrated areas used to construct analytical response curves. Limits of detection using this relatively simple atomic emission system are on the order of tens of nanograms for sample masses of ∼50 μg. Mass spectrometric monitoring of introduced caffeine particles and a mixture of polycyclic aromatic hydrocarbons (PAHs) illustrates the ability of the glow discharge plasma to produce high-quality, library (electron impact) searchable mass spectra of molecular species while also yielding isotopic identification of elemental components of the UPM. Limits of detection for Fe in the NIST SRM are on the order of 175 ng of material, equivalent to ∼7 ng of analyte Fe. It is believed that the small size, low power consumption, ease of operation, and multimode sampling capabilities (AES/MS) of the particle beam-glow discharge (PB-GD) apparatus hold promise for applications in continuous monitoring and discrete particle sampling.
authors.affiliation: Howard L. Hunter Chemical Laboratories, Department of Chemistry, Clemson University, Clemson, South Carolina 29634-1905.
authors.forename: R K
authors.initials: RK
authors.lastname: Marcus
authors.forename: M A
authors.initials: MA
authors.lastname: Dempster
authors.forename: T E
authors.initials: TE
authors.lastname: Gibeau
authors.forename: E M
authors.initials: EM
authors.lastname: Reynolds