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HIGH-ENERGY X-RAY FLUORESCENCE of this sample using the L lines, as can be seen in Figure 5.5.9(b). In addition, without such light elements, possibly 14 rare earth elements (from La to Lu except for Pm) and 42 peaks (L , L 1 , and L 2 lines for each element if we neglect the L line) are present in the XRF spectrum within the small energy region of 5.288 keV (=9.938 4.650). In contrast, in the energy region above 20 keV, there are no peaks other than the K lines of the heavy elements. Moreover, the energy difference between La K 1 (33.4418 keV) and LuK 1 (52.3889 keV) is ca. 19 keV, which is large enough to distinguish each rare earth element under the resolution of a pure Ge SSD, as is demonstrated in Figure 5.5.9(a). Certi ed values for the rare earth elements have not been reported for SRM612 glass, but information values (in ppm) are given as follows: Ag(21), Ba(41), La(36), Ce(39), Nd(36), Sm(39), Eu(36), Gd(39), Dy(35), Er(39), and Yb(42). The intensity of the peak of each element in Figure 5.5.9(a) appears to be qualitatively consistent with these information values. This suggests that the present technique is applicable for the nondestructive total determination of rare earth elements as well as for other heavy elements, such as Hf and Ta, at the ppm level.19

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PARABOLIC COMPOUND REFRACTIVE X-RAY LENSES the -XRF maps alone, it is not possible to judge whether the spots of accumulation of the heavy metals are situated on the particle surface (ie most prone to leaching) or are present at some depth within the particle (where they might be more shielded from chemical attack by water) To further understand the speciation of Cd in single y ash particles, the oxidation state and the chemical surroundings of Cd ions were studied by -XAS in the areas of the particles showing a higher Cd concentration -XAS spectra of pure Cd compounds such as Cd, CdO, CdSO4 , CdS, CdCl2 , CdBr2 pellets were measured prior to the single particle analysis, normalized and reported in Figure 3411(a).

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Comparisons of XAS spectra for y ashes and for reference compounds show that in all the particles studied Cd is present in oxidation state +2 instead of metallic form This can be explained by the oxidizing conditions experimented by the toxic metals after volatilization during combustion The -XAS spectra of the hot-spots of the particles were also expressed mathematically as a Linear Combination (LC) of XAS t vectors, using the measured absorption data of the Cd reference compounds The -XAS spectra of one of the two hot-spots , within particle 6, is shown in Figure 3411(b) The comparison between the linear combinations of the standard spectra and the measured XAS-spectra of the Cd hot-spots allow the concentrations to be estimated of the possible Cd compounds in those spots, eg.

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in the case of the spot a in particle 6, Cd is present as an admixture of CdSO4 (70 %), CdO (19 %) and CdCl2 (11 %) with over 90 % con dence level in the tting process In all the spots analysed, Cd was always present as a combination of just CdSO4 , CdCl2 and CdO Thus, it can be seen that the Cd in MSW y ashes is present as water soluble species (CdCl2 and CdSO4 ) up to 86 % and 76 %, respectively These results con rm what was found by XRF mapping and agree with earlier studies70,71 Such metal speciation would make the management of this lter ash problematic with respect to their possible leaching On the other hand this is not a conclusive identi cation because the spectra.

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