Individual aerosol particles (n = 1170) collected at work stations in a nickel refinery were analyzed by wavelength-dispersive electron-probe microanalysis. By placing arbitrary restrictions on the contents of sulfur and silicon, the particles could be divided into four main groups. Scanning electron images indicated that most of the particles examined were relatively small (< or = 2 microm, equivalent projected area diameter), and that their morphology suggested formation from a melt. There was an absence of well-defined phases and simple stoichiometries, indicating that exposures to pure substances such as nickel subsulfide or specific oxides appeared not to occur. Although the elemental composition of particles varied greatly, a rough association was evident with the known elemental content of the refinery intermediates. The implications of the findings for aerosol speciation measurements, toxicological studies and interpretation of adverse health effects are explored.
Aerosol particles with aerodynamic diameters between 0.18 and 10 microm were collected in the workroom air of two aluminium smelter potrooms with different production processes (Soderberg and Prebake processes). Size, morphology and chemical composition of more than 2000 individual particles were determined by high resolution scanning electron microscopy and energy-dispersive X-ray microanalysis. Based on chemical composition and morphology, particles were classified into different groups. Particle groups with a relative abundance above 1%(by number) include aluminium oxides, cryolite, aluminium oxides-cryolite mixtures, soot, silicates and sea salt. In both production halls, mixtures of aluminium oxides and cryolite are the dominant particle group. Many particles have fluoride-containing surface coatings or show agglomerations of nanometer-sized fluoride-containing particles on their surface. The phase composition of approximately 100 particles was studied by transmission electron microscopy. According to selected area electron diffraction, sodium beta-alumina (NaAl(11)O(17)) is the dominant aluminium oxide and cryolite (Na(3)AlF(6)) the only sodium aluminium fluoride present. Implications of our findings for assessment of adverse health effects are discussed.
The oxidation state of sulfur has been determined by measuring the energy shift of the S K(alpha) line by wavelength-dispersive electron-probe microanalysis. On flat polished samples the energy shift between sulfate (S(+6)) and sulfide (S(-2)) was 1.3 eV, in good agreement with previous literature data. The observed energy shift of the S K(alpha) line is dominated by the change of the valence state of sulfur--the effects of co-ordination geometry and nearest neighbours are small. The relationship between the energy shift of the S K(alpha) line and the oxidation number of sulfur is linear, to a first approximation. The effect of particle geometry on the position of the S K(alpha) line is usually small and introduces an error of approximately half an oxidation number. The apparent sulfur valence states observed for individual aerosol particles from work places in a nickel refinery are highly variable and most probably result from different mixtures of the two end-members sulfide and sulfate.
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