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Instruments / Technical Area	Publication Details	Published
B18-Core EXAFS	Speciation of toxic metals in metal finishing filter cake by X-ray absorption spectroscopy Dan Ting Chen , Amitava Roy , Anna Bogush , Julia A. Stegemann Journal Of Environmental Management 360 DOI: 10.1016/j.jenvman.2024.120994 Diamond Proposal Number(s): [11156, 16153] Show Abstract ▼ Abstract: The speciation of Cr, Zn, Cu and Pb in two metal finishing filter cakes (TX and ST) was investigated by X-ray absorption spectroscopy (XAS) complemented by X-ray fluorescence (XRF) and X-ray diffraction (XRD). XRF showed that concentrations of Cr, Zn, Cu and Pb were 1.4%, 0.19%, 0.20% and 0.01%, respectively, in TX, and 12.6%, 3.3%, 1.3% and 0.21% in ST. No crystalline phases were detected in TX by XRD whereas ST was dominated by calcite. Cr and Fe K edge XAS showed Cr to be trivalent and octahedrally coordinated, co-precipitated with Fe as CrxFe1-x-(oxy)hydroxides in both filter cakes. Zn, P and Ca K edge XAS showed that 2ZnCO3∙3Zn(OH)2 and Zn3(PO4)2 were the dominant zinc-containing phases, with combined tetrahedral and octahedral coordination; Zn phases were slightly more crystalline in TX than ST. Pb L3 edge X-ray absorption near edge spectroscopy (XANES) found that Pb was likely adsorbed on amorphous SiO2. Cu, Si and S K edge XAS showed that all Cu was divalent, and the dominant copper phases were found to be Cu2Cl(OH)3, Cu(OH)2 and CuSO4·5H2O for ST, whereas Cu appeared to adsorb to amorphous SiO2 for TX, which contained much less Pb. Cr is thus immobilized in the filter cakes in a phase with low solubility at environmentally feasible pH values, whereas Zn, Cu and Pb could be released when the pH decreases below 8 or above 11. These findings are significant for the development of waste management regulations and/or metal recovery methods (e.g., hydro/pyrometallurgy).	Jun 2024
B18-Core EXAFS	Speciation of toxic pollutants in Pb/Zn smelter slags by X-ray Absorption Spectroscopy in the context of the literature Dan Ting Chen , Amitava Roy , Yu Qian Li , Anna Bogush , Wing Yin Au , Julia A. Stegemann Journal Of Hazardous Materials 8 DOI: 10.1016/j.jhazmat.2023.132373 Diamond Proposal Number(s): [11156] Open Access Show Abstract ▼ Abstract: Pb/Zn smelter slag is a hazardous industrial waste from the Imperial Smelting Process (ISP). The speciation of zinc, lead, copper and arsenic in the slag controls their recovery or fate in the environment but has been little investigated. X-ray Absorption Spectroscopy (XAS) was applied to this complex poorly crystalline material for the first time to gain new insights about speciation of elements at low concentration. Zn, Cu, As K-edge and Pb L3-edge XAS was carried out for a Pb/Zn slag from a closed ISP facility in England, supported by Fe, S and P K-edge XAS. Results are presented in the context of a full review of the literature. X-ray fluorescence showed that concentrations of Zn, Pb, Cu and As were 8.4, 1.6, 0.48 and 0.45 wt.%, respectively. Wüstite (FeO) was the only crystalline phase identified by X-ray diffraction, but XAS provided a more complete understanding of the matrix. Zn was found to be mainly present in glass, ZnS, and possibly solid solutions with Fe oxides; Pb was mainly present in glass and apatite minerals (e.g., Pb5(PO4)3OH); Cu was mainly speciated as Cu2S, with some metallic Cu and a weathering product, Cu(OH)2; As speciation was likely dominated by arsenic (III) and (V) oxides and sulfides.	Aug 2023
B18-Core EXAFS	Changes in composition and lead speciation due to water washing of air pollution control residue from municipal waste incineration A. A. Bogush , J. A. Stegemann , A. Roy Journal Of Hazardous Materials DOI: 10.1016/j.jhazmat.2018.08.051 Diamond Proposal Number(s): [11156] Open Access Show Abstract ▼ Abstract: Changes in elemental and mineralogical composition, and lead speciation, of air pollution control residue (APCR) from municipal solid waste incineration, due to treatment by water washing, were investigated in this work and are reported in the context of a review of the literature. Water washing was shown to substantially modify the nature of APCR by: 1) removing 23% dry mass soluble salts to disagglomerate particles and significantly reduce concentrations of the associated major elements, and increase concentrations of insoluble matrix elements and potential pollutants; and 2) respeciating elements to form new phases. X-ray absorption near edge spectroscopy (XANES) showed that the 500 mg/kg of Pb in raw and washed APCR were comprised mainly of Pb-glass, with some PbSO4, and small amounts of PbO and PbCl2. Semi-quantitative linear combination fitting suggests that the glass in the APCR may be unstable and release Pb under the alkaline pH of water washing, to reprecipitate as PbO. Chemical analysis suggests that some Pb may be removed by washing. Scientific understanding of the composition of raw and washed APCR, and particularly the speciation of potentially toxic metals, such as Zn and Pb, can help in developing effective element recovery and residue treatment, utilization or disposal strategies.	Aug 2018

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