Abstract: Airborne dust particles were collected in a return airway of a South African gold mine using a 7-stage, single-orifice cascade impactor. Between 70 and 130 individual particles were analysed on each stage using automated electron-probe x-ray microanalysis (EPXMA). Particle size and shape parameters are given for different classes of particles sorted by elemental composition. Silicon-rich particles are the most abundant overall, while chlorine-rich particles dominate (up to 80%) in the range 0.21.0 μm. It is shown that EPXMA characterisation of particles can be used to infer relative contributions of various particle sources and dust generating processes to the total dust concentrations in mine atmospheres. An understanding of the nature and source of particles is essential for any source control strategy. We conclude that the EPXMA technique merits inclusion in the repertoire of techniques used for characterising underground dust.

Abstract: A nonurban base line has been established for nine trace element constituents of aerosol particles as a function of particle size at ground level sampling stations in north Florida up to 50 km from the Gulf of Mexico. The particle size range 0.25- to >4-μm aerodynamic diameter was investigated by cascade impactor sampling and elemental analysis by proton-induced X ray emission. By using a strategy of sampling at urban, forest, and coastal locations and by choosing approximately 48-hour sample averaging intervals the potential dependence of the base line levels both on local pollution and natural sources and on local particle size specific aerosol removal processes could be evaluated. It is found that elements contained in the largest particles, especially those of >4 μm, display the greatest degree of average concentration difference between sites, a result suggesting short atmospheric residence times and the importance of local dispersion sources and atmospheric cleansing processes in regulating the particle concentrations in air. Elements contained in particles of <2-μm diameter show little average concentration difference between sites unless they are influenced by local pollution sources, a finding suggesting that their concentrations in air are regulated by large-scale sources and transport processes. Sulfur in the smallest particles shows a marked constancy of concentration, but it may be modified in the largest particle size ranges in relation to proximity to the seacoast. No evidence is found for dependence of particulate sulfur concentrations on local pollution sources. K, Ca, Ti, Fe, and Zn appear to be regulated in the main by terrestrial source processes, and Cl by marine source processes, but Br and Pb appear to be accounted for adequately by assuming automotive fuel combustion as their major source. Limited data obtained for V indicate that it may vary considerably with fluctuations in aerosol transport from oil-fired electric power plant sources in the region. Limited additional data also suggest that Mn is derived from sources of natural terrestrial composition. In view of these findings, certain criteria may be set for the design of a meaningful nonurban aerosol monitoring network.

Abstract: The ArmstrongBuseck correction for absorption effects in electron probe x-ray microanalysis of particles considers seven specific particle shapes, and for these geometries exact correction equations are used. This procedure implies that the analyst has to associate the particle to be analysed with a certain particle type; an arbitrary relative thickness is sometimes assumed. A theoretical study was made of this absorption correction as a function of the particle composition, type and thickness for micrometre-sized particles. It appears that a correct choice of the particle type is critical. However, when the analytical results are normalized to 100%, the differences between the models are much less pronounced, and it is justified to assume a spherical model in all cases.

Abstract: Folding aerosol loaded filters in two with the loaded side inwards during the X-ray analysis not only reduces possible filter heterogeneity effects and improves sample protection, but also increases the sensitivity and renders filter paper absorption corrections simple and more accurate in many instances. It is shown that folding an aerosol loaded Whatman filter paper during Kα X-rays counting leads to an increased sensitivity for all elements up from calcium, scandium or titanium (depending on the sensitivity definition and on the aerosol load) and for all elements up from phosphorus, sulphur or chlorine in the case of the Nuclepore filter. Although the absorption by the filter, into which the aerosol penetrates to some extent, is always more important in the sandwich than in the usual geometry, the dependence of the absorption correction on the usually unknown average deposition depth is less pronounced. Assuming all the aerosol material to be collected at the very surface of the filter and hence being present in the centre of the sandwich to be analysed, leads to an extremely simple filter paper absorption correction which is less prone to uncertainties than more sophisticated corrections in the usual geometry requiring additional measurements. This is the case for all elements up from potassium on Whatman filters and up from phosphorus on Nuclepore filters.

Abstract: A variety of samples, collected from different historical buildings and monuments throughout Belgium, were thoroughly studied, using several trace- and micro-analysis techniques. Thin sections of stones and mortar joints were characterized by means of electron probe X-ray microanalysis (EPXMA). The morphological appearance of the surface weathering crust and the possible presence of non-innate particles in the crust were elucidated using petrographical and electron microscopy. Quantitative characterization of the total chemical composition of the crust surface layer and underlying layer was performed by energy-dispersive X-ray fluorescence, and by ion chromatography and atomic absorption spectrometry for the leachable components. Special attention was also paid to the chemical composition of rain and air at the particular sampling sites. The element distribution in the transition zone between the weathering crust and the original stone material was found to vary greatly amongst the different samples analyzed. Detailed EPXMA measurements on pieces of the weathering crust showed remarkable differences in morphology and composition between the surface and the underlying layer, and provided information about the presence of fly-ash and soil dust particles in the crust. Except for crusts from the city of Brussels, which were all very high in sulphate, the samples appeared to contain very variable sulphate contents; very local micro-climate and environmental conditions at a particular site are more important in determining the weathering condition of the building stones than the local air pollution situation. Bulk analytical characterization further showed, in all the crust samples studied, a very small contribution of nitrogen- and chlorine-containing weathering products, in contrast to sulphur-containing weathering salts.

Abstract: Adding 20mg of 1-(2-pyridylazo)-2-naphthol (PAN) to a water sample at 70°, and filtering off the precipitate after cooling, gives efficient preconcentration prior to X-ray fluorescence analysis of water. Up to the capacity of about 100 μeq of PAN used, the trace metal recoveries are around 90% or higher for Cr3+, Mn2+, Ni2+, Cu2+, Zn2+, Hg2+ and Eu3+, and above 70% for many other ions. The recovery yields usually do not vary critically with pH in the neutral pH-range, and are practically independent of the sample salinity, sample volume and trace-metal concentration. Enrichment factors as high as 2 × 105 can be achieved. Counting statistics would then allow detection limits of 0.03 ppM. The blank levels in commercial PAN, however, lead to typical detection limits of about 1 ppm. The coefficient of variation is typically in the 510% range at the 10-ppM level. The accuracy and applicability of the procedure are illustrated by comparative analyses on samples of synthetic solutions, river and drinking water.

Abstract: For trace analyses of environmental waters, spark-source mass-spectrometry has been combined with a preconcentration procedure involving chelation of the dissolved trace elements with oxine and subsequent adsorption of the oxinates and naturally occurring organic and colloidal metal species onto activated carbon. The activated carbon is filtered off and ashed at low temperature. The residue is dissolved, an internal standard and pure graphite are added and, after drying, the electrodes are prepared. The photographically recorded mass spectrum is evaluated by a suitable computer routine. The error of the procedure is around 30%. While this preconcentration and analysis procedure is capable of measuring about 40 elements quantitatively, in practice 1025 trace elements are determined simultaneously above the 0.1-μg/l. detection limit, as is illustrated by analyses of drinking water, surface and ground water samples. Although a sophisticated technique, SSMS can be considered for regular panoramic survey analyses.

Abstract: Triammonium aurin tricarboxylate (aluminon) has been used to localize aluminum in 2 μm sections of undecalcified, methyl methacrylate embedded bone obtained from patients with terminal chronic renal failure. Aluminum appeared in four cases as bright red lines at the mineralized-bone boundary. In two cases, however, purplish lines were found and one patient showed red as well as purplish lines. Laser microprobe mass analysis (LAMMA) identified aluminum at the location of the red lines and both aluminum and iron at the purplish lines. Furthermore, both iron and aluminum were found in histiocytic bone marrow cells, which showed brownish aluminon staining. It appears that when aluminum and iron occur together, aluminon staining may yield aberrant results. This study shows that LAMMA can be used for the identification of elements sought by histochemical methods and thus permits the evaluation of their staining effects.

Abstract: Sixty-two samples of total sediments and the separated clay/silt size fractions were analysed by energy-dispersive X-ray fluorescence spectrometry to evaluate the pollution level and the trends in samples collected along the Belgian coast over a period of 6 yr and at four stations located in the Scheldt estuary where two of these were sampled periodically for 4 yr. Three correction methods for grain size effects were applied, either to the bulk sediment samples or to the clay/silt size fractions, and the results were compared. Local variations on the concentrations in some of the elements determined were used to establish whether they result from an anthropogenic or natural origin. The level of pollution was assessed as a function of the location, sampling date, and depth.