Nanosize-controllable Cu, Ag, Pd, Ni, CuPd alloy and Cu-Ag bimetal encapsulated in inert carbon shells can be synthesized by carbonization of metal-cyclodextrin complexes with a remarkable capability of experimentally determining the size-dependent melting temperature depression of many metal or alloy nanoparticles.
Speciation of copper-humic substances (HS) in the electrokinetic remediation (EKR) of a contaminated soil was studied by in situ extended X-ray absorption fine structure (EXAFS) and X-ray absorption near edge structure (XANES) spectroscopies. The least-square fits of the XANES spectra suggested that the main Cu species in the contaminated soil were Cu-HS (50%), CuCO(3) (28%), Cu(2)O (11%), and CuO (11%). The Cu-HS in the contaminated soil possessed equatorial and axial Cu-O bond distances of 1.94 and 2.17 A with coordination numbers (CNs) of 3.6 and 1.4, respectively. In the EKR process, the axial Cu-O bond distance in the Cu-HS complexes was increased by 0.15 A, which might be due to a ligand exchange of the Cu-HS with H(2)O molecules in the electrolyte. After 180 min of EKR, about 50% of the Cu-HS complexes (or 24% of total Cu) in the soil were dissolved and formed [Cu(H(2)O)(6)](2+) in the electrolyte, 71% (or 17% of total Cu in the soil) of which were migrated to the cathode under the electric field (5 V/cm). This work exemplifies the use of in situ EXAFS and XANES spectroscopies for speciation studies of Cu chelated with HS in the contaminated soil during EKR.
Environmental context. Very fine phosphor ashes are discharged from particulate collection systems (such as bag houses) in the cathode ray tube or television disassembling processes. Effective recovery of ZnO and ZnS nanoparticles from the phosphor ash can be achieved by extraction with a room temperature ionic liquid. By synchrotron radiation X-ray absorption spectroscopy, the obtained molecular scale data turn out to be very useful in revealing speciation of zinc in the extraction process, which also facilitates the development of a simple nanoparticle recovery method.
Abstract. An effective, simple method has been developed for the recovery of ZnO and ZnS nanoparticles from hazardous phosphor ash waste. Experimentally, zinc (77%) in the phosphor ash (that contains mainly zinc (91%)) can be recovered by extraction with a room temperature ionic liquid (RTIL) ([C4mim][PF6], 1-butyl-3-methylimidazolium hexafluorophosphate). Component fitted X-ray absorption near edge structure (XANES) spectra of zinc indicate that metallic zinc (Zn) (9%) in the phosphor ash can be dissolved to form a Zn2+–1-methylimidazole ([mim]) complex during extraction with the RTIL. ZnS and ZnO nanoparticles (60–61%) can also be extracted from the phosphor. Over the 298–523 K temperature range, desired ZnO/ZnS ratios (0.3–0.6) can be obtained since interconversion of ZnS to ZnO in the RTIL is temperature dependent. The Fourier transformed extended X-ray absorption fine structure (EXAFS) data also show that the nanosize ZnS extracted in the RTIL possesses a Zn–S bond distance of 2.33 Å with coordination numbers (CNs) of 3.6–3.7. At 523 K, in the RTIL, ~30% of the ZnS is oxidised to form octahedral ZnO (with a bond distance of 2.10 Å and a CN of 6.1) that may coat the surfaces of the ZnS nanoparticles. This work exemplifies the utilisation of X-ray absorption spectroscopy (EXAFS and XANES) to reveal speciation and possible reaction pathways in a nanoparticle extraction process (with a RTIL) in detail.
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