Le. Giblin et al., X-RAY CONTINUUM DISCRIMINATION TECHNIQUE FOR THE ENERGY-DISPERSIVE ANALYSIS OF FINE PARTICLES, Analytical chemistry, 65(24), 1993, pp. 3576-3580
Discrimination criteria are proposed for selecting irregularly shaped
and unpolished fine grains for quantitative analyses by energy dispers
ive X-ray (EDS) spectroscopy. The basic principle is that the energy d
istribution of the continuum or background radiation is a direct indic
ation of the orientation of the particle surface at the point of analy
sis. Background spectra were collected from pure elements in various g
eometric configurations and orientations from which it was observed th
at the low-energy (<4 keV) portion of the spectra was most sensitive t
o the orientation of the specimen surface, showing a strong increase i
n intensity with increasing specimen tilt up to about 40-degrees. A si
mple ratio of low-high-energy windows in the background radiation prov
ided an adequate indication of the orientation of the particle surface
. Combination of this discrimination criterion with the requirement th
at the analytical total be 60 wt % or better provided oxide analyses f
rom garnet and anorthite particles that were within 7% relative standa
rd deviation (RSD) for oxides in the 10-40 wt % range and within 9% RS
D for oxides in the 1-10 wt % range.