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Instruments / Technical Area	Publication Details	Published
I18-Microfocus Spectroscopy	Reclamation of available phosphorus and separation of heavy metals from sewage sludge via FeCl3-assisted electrokinetic treatment and pyrolysis Xutong Wang , Huwei Li , Junxia Wang , Wolfram Buss , Anna Bogush , Ondrej Masek , Youjun Zhang , Fan Yu , Beibei Yan , Zhanjun Cheng , Xiaoqiang Cui , Guanyi Chen , Konstantin Ignatyev Journal Of Environmental Management 387 DOI: 10.1016/j.jenvman.2025.125882 Diamond Proposal Number(s): [32515] Show Abstract ▼ Abstract: Recycling of sewage sludge and the endogenous phosphorus (P) is a promising strategy for sustainable development, while the disposal of heavy metals (HMs) in sewage sludge and the recovery of targeted P species remain challenges. An innovative method coupling electrokinetic treatment with pyrolysis was proposed in the present study to achieve the effective reclamation of available P and the separation of HMs from sewage sludge. The pristine and FeCl3-assisted electrokinetic treatment were employed for the removal of HMs from sewage sludge and to modify the P species, and the subsequent pyrolysis (300–700 °C) was conducted for the recovery of available P along with the production of biochar. The X-ray absorption near-edge spectroscopy (XANES), 31P liquid nuclear magnetic resonance (NMR) spectroscopy, and sequential chemical extraction were used to systematically determine the evolution of P during the combined treatment of sewage sludge. 19.69–24.80 % of Ni, Cu, and Zn were removed from sewage sludge after pristine electrokinetic treatment, and the HM removal efficiency was further elevated to 47.01–56.86 % with the assistance of FeCl3. Consequently, in comparison with the raw sewage sludge-derived biochars (SBs), the biochars derived from FeCl3-assisted electrokinetic treated sewage sludge (FESBs) contained much lower HM contents and showed higher stability of HMs. The FeCl3-assisted electrokinetic treatment converted alkaline biochars dominated by poorly soluble Ca-phosphates into neutral to slightly acidic biochars dominated by Al/Fe-associated phosphates. This transformation greatly improved the available P concentrations determined by diffusive gradients in thin film in FESBs by 0.6–1.3 folds compared to untreated SBs. Therefore, coupling FeCl3–assisted electrokinetic treatment with pyrolysis could be a promising strategy to achieve the reclamation of available P and the separation of HMs from sewage sludge.	Jul 2025
I18-Microfocus Spectroscopy	Spatial variability of metal(loid) leaching from coastal colliery wastes under freshwater and saline water conditions Catherine J. Gandy , Ian T. Burke , Patrick Byrne , Nick Cooper , Richard A. Crane , Karen A. Hudson-Edwards , William M. Mayes , Patrizia Onnis , Alex L. Riley , Adam P. Jarvis Journal Of Environmental Management 376 DOI: 10.1016/j.jenvman.2025.124489 Diamond Proposal Number(s): [29808] Open Access Show Abstract ▼ Abstract: Historical disposal of coal mine wastes in the coastal zone has left a significant environmental pollution legacy. Climate change is increasing the likelihood that erosion of these wastes will lead to release of metal(loid)s to coastal environments. Whilst previous research has focussed on the generation of acidic, metal-rich waters from coal mine wastes in freshwater environments, a comprehensive investigation of metal(loid) leaching from such wastes in the coastal zone has not been undertaken. This study investigated the leaching behaviour of coal mine wastes under freshwater and saline conditions and determined the impacts of spatial heterogeneity of waste composition on such behaviour. The degree of leaching varied considerably within and between sites due to the heterogenous nature of the waste. Leachate pH varied from 1.80 to 6.99 with acidic leachates particularly enriched in Fe (≤17,000 mg/kg dry waste) and sulfate (≤48,000 mg/kg dry waste) due to dissolution of acid sulfate phases. Dissolution of Fe and Mn oxides, hydroxides and oxyhydroxides also led to release of surface adsorbed metal(loid)s such as As (≤21 mg/kg dry waste), Zn (≤86 mg/kg dry waste) and Cu (≤14 mg/kg dry waste). Adsorption of As to high surface area minerals was confirmed by X-ray Absorption Near Edge Spectroscopy (XANES) analysis. Metal(loid) release was typically lower in the presence of seawater than deionised water due to the greater pH buffering capacity of seawater. This research provides an insight into the considerable challenges faced by coastal managers globally as they seek to mitigate the risks from such legacy pollution.	Mar 2025
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

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