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Heavy metal adsorption on iron oxide and iron oxide-coated silica ...

Heavy metal adsorption on iron oxide and iron oxide-coated silica ...

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43Lin-edge, from 8,133 to 8,884 eV over the Ni K-edge, <strong>and</strong> from 6,912 to 7,857 eV overthe Fe K-edge. Pb, Ni, <strong>and</strong> Fe foils were used as references for energy calibrati<strong>on</strong>. Atleast five scans for Fe <strong>and</strong> typically —20 scans for Pb <strong>and</strong> Ni were collected. The analysiswas carried out <strong>on</strong> the averaged data to improve signal statistics. All EXAFS data werecollected at room temperature. XAS data for reference compounds were collected intransmissi<strong>on</strong> mode. Both transmissi<strong>on</strong> <strong>and</strong> fluorescence data were collected for thehydrated i<strong>on</strong> in a <str<strong>on</strong>g>metal</str<strong>on</strong>g> nitrate soluti<strong>on</strong> in order to address self-absorpti<strong>on</strong> (Tröger et al.1992).The XAS data were analyzed with WinXAS 2.3 (Ressler, 1998) <strong>and</strong> followedst<strong>and</strong>ard procedures (Bunker <strong>and</strong> Sayers, 1988). For each scan, the background wasfitted with a linear polynomial through the pre-edge regi<strong>on</strong> <strong>and</strong> subtracted. The edgejump of the background-corrected XAS spectra was then normalized to <strong>on</strong>e by refining100-200 eV above the edge with a zero order polynomial <strong>and</strong> normalizing the spectra tothe ordinate value of this polynomial. The energy threshold (E0) of the absorpti<strong>on</strong>spectrum was determined from the first inflecti<strong>on</strong> point of the edge regi<strong>on</strong> <strong>and</strong> was usedto c<strong>on</strong>vert the absorpti<strong>on</strong> spectrum from energy to k space. A cubic spline functi<strong>on</strong> wasapplied to account for the isolated atomic absorpti<strong>on</strong> μ0(E). EXAFS functi<strong>on</strong> (x(k)) wasobtained after subtracting ,u0(E) from the absorpti<strong>on</strong> of the atom in c<strong>on</strong>densed matter.The x(k) data were weighted by k 3 to enhance the higher k-space data <strong>and</strong> then Fouriertransformed using the Bessel window functi<strong>on</strong> to produce the radial structural functi<strong>on</strong>(RSF). The RSF was not corrected for phase shift. EXAFS fitting of the RSF wasc<strong>on</strong>ducted using theoretical phase shift <strong>and</strong> amplitude functi<strong>on</strong>s calculated by FEFF 7

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