Analysis of size-fractionated coal combustion aerosols by PIXE and other analytical techniques

Particle-induced X-ray emission (PIXE) analysis, instrumental neutron activation analysis (INAA) and inductively coupled plasma mass spectrometry (ICP-MS) were used to study the chemical composition of size-fractionated in-stack fly-ash particles emitted during coal combustion. The samples were collected before the electrostatic precipitator at a gas temperature of 120°C during the combustion of Venezuelan coal in a 81 MW capacity circulating fluidized bed boiler. The sampling device consisted of a Berner low pressure impactor, which was operated with a cyclone precutter. The Nuclepore polycarbonate foils, which were used as collection surfaces in the low pressure impactor, were analyzed by the three techniques and the results of common elements were critically compared. The PIXE results were systematically lower than the INAA data and the percentage difference appeared to be stage-dependent, but virtually independent upon the element. The discrepancies are most likely due to bounce-off effects, particle reentrainment and other sampling artifacts, which may make that a fraction of the aerosol particles is deposited on the impaction foils outside the section analyzed by PIXE. However, by resorting to a “mixed internal standard” approach, accurate PIXE data are obtained. Also in the comparison between the ICP-MS and the INAA data significant discrepancies were observed. These are most likely due to incomplete dissolution of the particulate material and in particular of the alumino-silicate fly-ash matrix, during the acid digestion sample preparation step for ICP-MS. It is suggested that a comparison between ICP-MS data of acid digested samples and INAA can advantageously be used to provide speciation information on the various elements. Selected examples of size distributions are presented and briefly discussed.