Application of synchrotron microprobe methods to solid-phase speciation of metals and metalloids in house dust.

Determination of the source and form of metals in house dust is important to those working to understand human and particularly childhood exposure to metals in residential environments. We report the development of a synchrotron microprobe technique for characterization of multiple metal hosts in house dust. We have applied X-ray fluorescence for chemical characterization and X-ray diffraction for crystal structure identification using microfocused synchrotron X-rays at a less than 10 µm spot size. The technique has been evaluated by application to archived house dust samples containing elevated concentrations of Pb, Zn, and Ba in bedroom dust, and Pb and As in living room dust. The technique was also applied to a sample of soil from the corresponding garden to identify linkages between indoor and outdoor sources of metals. Paint pigments including white lead (hydrocerussite) and lithopone (wurtzite and barite) are the primary source of Pb, Zn, and Ba in bedroom dust, probably related to renovation activity in the home at the time of sampling. The much lower Pb content in the living room dust shows a relationship to the exterior soil and no specific evidence of Pb and Zn from the bedroom paint pigments. The technique was also successful at confirming the presence of chromated copper arsenate treated wood as a source of As in the living room dust. The results of the study have confirmed the utility of this approach in identifying specific metal forms within the dust.

Fracture wall cements and coatings from two clayey till aquitards.

Secondary minerals occurring at the faces of fractures, the only reliable visual evidence of the presence of hydraulically conductive fractures in clayey unlithified aquitards, have been characterized for two uncontaminated field sites, Dalmeny, Saskatchewan, and Laidlaw, Ontario. Preliminary identification of secondary minerals and their variations with depth was made using a Munsell Color Chart. Subsequent microscopic analyses (petrography, electron microprobe analysis, scanning electron microscopy, and X-ray diffraction) were used to identify iron-oxide mineralogy. Iron oxides were identified as goethite, ferrihydrite, and hematite at Dalmeny, where they occur to depths of 10 to 15 m, and goethite and ferrihydrite at Laidlaw, observed to depths of 7 m. In both cases, the identification of ferrihydrite was tentative due to the problems of small sample size and peak overlap in X-ray diffraction. The iron oxides do not form coatings on the surfaces of the fractures as had been previously thought; rather they form cements linking the matrix grains. Thus there is potential for decreased permeability and increased surface reactivity parallel to and inward from the fracture faces. The pattern of iron-oxide distribution suggests that the youngest deposits, and those with the greatest surface reactivity and potential for contaminant retardation, are found at greatest depths in the fractures. Manganese oxides form in isolated clusters in larger pores and indentations, although the exact manganese minerals could not be firmly identified.