title: Reliability of chemical microanalyses for solid waste materials.
abstract: The investigation of solid speciation of metals and metalloids is required for accurate assessment of the hazardous properties of solid waste materials from high-temperature technologies (slag, bottom ash, fly ash, air-pollution-control residues). This paper deals with the problem of reliability of microanalyses using a combination of electron microprobe analysis (EPMA) and scanning electron microscopy (SEM) only. These methods do not permit to detect nanophases in host-crystals and lead to erroneous interpretation of analytical results, considering the elements of nanophases as belonging to the crystal structure of the main phase. More detailed analysis using transmission electron microscopy (TEM) on foils prepared by focused ion beam (FIB) can be used to solve this analytical problem. In this study, lamellar aggregates of potassium-rich clinopyroxenes were detected in copper smelting slags by a combination of SEM and EPMA. However, FIB-TEM indicated the presence of leucite inclusions (tens to hundreds nm in size) within the clinopyroxene lamellae. Based on examples from smelting slags and other solid waste materials, recommendations for standard SEM and EPMA applications and the need for methods with higher resolution for mineralogical investigation of waste materials are discussed.
authors.affiliation: Institute of Geochemistry, Mineralogy and Mineral Resources, Charles University in Prague, Faculty of Science, Albertov 6, 128 43 Prague 2, Czech Republic. ettler@natur.cuni.cz
authors.forename: Vojtěch
authors.initials: V
authors.lastname: Ettler
authors.forename: Zdenek
authors.initials: Z
authors.lastname: Johan
authors.forename: Martina
authors.initials: M
authors.lastname: Vítková
authors.forename: Roman
authors.initials: R
authors.lastname: Skála
authors.forename: Marek
authors.initials: M
authors.lastname: Kotrlý
authors.forename: Gerlinde
authors.initials: G
authors.lastname: Habler
authors.forename: Mariana
authors.initials: M
authors.lastname: Klementová
mesh_terms: D004577:Electron Probe Microanalysis; D015386:Hazardous Substances / Q000032:analysis*; D008855:Microscopy, Electron, Scanning; D046529:Microscopy, Electron, Transmission; D015203:Reproducibility of Results; D014961:X-Ray Diffraction
chemical_list: D015386:Hazardous Substances