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1.
The local and geometrical structure around gold (III) e.g., Au3+ ions in aqueous solution with different OH/Cl molar ratios, has been investigated by X-ray absorption spectroscopy (XAS). X-ray absorption near-edge structure (XANES) spectra of [AuCln(OH)4−n] solutions have been calculated and the multiple-scattering spectral features have been attributed to Cl d-states, axial water molecules and the replacement of Cl ligands by OH ligands. A square–planar geometry for [AuCln(OH)4−n] with two axial water molecules has been identified. Moreover, a spectral correlation between XANES features and the type of planar atoms has been identified. By extended X-ray absorption fine structure spectra (EXAFS), the planar Au bond distances in the solutions have also been determined, e.g., 2.28 Å for Au–Cl and 1.98 Å for Au–O, respectively. The same EXAFS analysis provides evidence that the peak at about 4.0 Å in solutions with the lowest OH/Cl molar ratio arises from collinear Cl–Au–Cl multiple-scattering contributions. For the first time, a complete detailed reconstruction of the hydration structure of an Au ion at different pH values has been achieved.  相似文献   
2.
Mn K-edge EXAFS spectroscopy of solid-solution samples encompassing the complete MnCO3–CaCO3 series shows that first-shell Mn–O distances deviate little from the 2.19-Å distance observed in pure MnCO3. Very slight lengthening is observed only in the limiting case of dilute Mn(II) calcite solid solutions, where the Mn–O distance is 2.21 Å. The observed nearly complete structural relaxation and the composition independence of the Mn–O distance are consistent with the Pauling model behavior of solid solutions, and agree with previous studies showing a high degree of relaxation around hetero-sized substituents in the calcite structure. Strain occurs through bond bending, which is facilitated by the exclusively corner-sharing topology of calcite. Observed distances from Mn to more distant neighbors show significant variation across the solid-solution series that resembles Vegard's law-type behavior but reflects averaging. The high degree of relaxation suggests modest enthalpies of mixing in the solution, consistent with calorimetric studies.  相似文献   
3.
张正阶  汪虹 《矿物岩石》1990,10(2):92-96
本文利用EXAFS方法对镁铝榴石、几种锰矿和不同铁含量的闪锌矿中有关阳离子的近邻结构进行了研究,得到了有关阳离子在相应矿物中的近邻结构参数.对闪锌矿的研究,得到了杂质Fe绝大部分以六配位的形式存在的结果,这与传统的观点不同;提出了闪锌矿不仅可作为地质温度计,还可能作为地质温度、压力变化记录仪的设想。  相似文献   
4.
Cement-based materials play an important role in multi-barrier concepts developed worldwide for the safe disposal of hazardous and radioactive wastes. Cement is used to condition and stabilize the waste materials and to construct the engineered barrier systems (container, backfill and liner materials) of repositories for radioactive waste. In this study, bulk-X-ray absorption spectroscopy (XAS) was used to investigate the uptake mechanism of Nd on the crystalline C–S–H phase 11 Å tobermorite in the presence of Zn (co-absorbing metal), and vice versa, as potential competitor under strongly alkaline conditions (pH = 12.5–13.3). The Zn and Nd concentration in all samples was 50,000 ppm, whereas the reaction times varied from 1 to 6 months.Extended X-ray absorption fine structure (EXAFS) data of the Nd LIII-edge indicate that the local structural environment of Nd consists of ∼7–8 O atoms at 2.42 Å, ∼7–8 Si at ∼3.67 Å and ∼5–6 Ca at ∼3.8 Å, and that this environment remains unchanged in the presence and absence of Zn. In contrary, Zn K-edge EXAFS data exhibit distinct differences in the presence and absence of Nd as co-absorbing element. Data analysis indicates that Zn is tetrahedrally coordinated (∼4 O at ∼1.96 Å) and the obtained structural data in the simultaneous presence of Nd and Zn are consistent with the formation of mixed Zn surface complexes and Zn bound in the interlayer remaining in these positions also with prolonged reaction times (up to 6 months). However, without the co-absorbing element Nd, strong structural changes in the uptake mechanisms of Zn are observable, e.g., after 3 month reaction time Zn–Zn backscattering pairs can be observed. These findings suggest that Nd has an influence on the incorporation of Zn in the tobermorite structure. In addition, the results of this study indicate that competitive uptake of metal cations with similar sorption behaviour by C–S–H phases can take place, deserving further attention in future assessments of the safe disposal of radioactive wastes in cement-based repositories.  相似文献   
5.
Immobilization of trace elements in contaminated soils by zero-valent iron (ZVI) is a promising remediation method, but questions about its long-term performance remain unanswered. To quantify immobilization and predict possible contaminant remobilization on long timescales detailed knowledge about immobilization mechanisms is needed. This study aimed at assessing the long-term effect of ZVI amendments on dissolved copper and arsenic in contaminated soils, at exploring the immobilization mechanism(s), and at setting up a geochemical model able to estimate dissolved copper and arsenic under different scenarios. Samples from untreated and ZVI-treated plots in two field experiments where ZVI had been added 6 and 15 years ago were investigated by a combination of batch experiments, geochemical modeling and extended X-ray absorption fine structure (EXAFS) spectroscopy. Dissolved copper and arsenic concentrations were described by a multisurface geochemical model with surface complexation reactions, verified by EXAFS. The ZVI remained “reactive” after 6–15 years, i.e. the dissolved concentrations of copper and arsenic were lower in the ZVI-treated than in the untreated soils. There was a shift in copper speciation from organic matter complexes in the untreated soil to surface complexes with iron (hydr)oxides in the ZVI-treated soil. The pH value was important for copper immobilization and ZVI did not have a stabilizing effect if pH was lower than about 6. Immobilization of arsenic was slightly pH-dependent and sensitive to the competition with phosphate. If phosphate was ignored in the modeling, the dissolution of arsenate was greatly underestimated.  相似文献   
6.
Extended X-ray absorption fine structure (EXAFS) spectroscopy and chemical analyses were combined to determine the Fe bearing minerals in recent lake sediments from Baldeggersee (Switzerland). The upper section of a laminated sediment core, deposited under eutrophic conditions, was compared to the lower part from an oligotrophic period. Qualitative analysis of FeK EXAFS agreed well with chemical data: In the oligotrophic section Fe(II)–O and Fe(III)–O specieswere present, whereas a significant fraction of Fe(II)–S sulfides was strongly indicated in the eutrophic part. A statistical analysis was performed by least square fitting of normalized reference spectra. The set of reference minerals included Fe(III) oxides and Fe(II) sulfides, carbonates and phosphates. In the oligotrophic regime no satisfying fit was obtained using the set of reference spectra, indicating that siderite (FeCO3) was not present in a significant amount in these carbonate-rich sediments. Simulated EXAFS spectra for a(Cax, Fe1-x)CO3solid solution allowed reconstructing the specificfeatures of the experimental spectra, suggesting that this phase was the dominant Fe carrier in the oligotrophic section of the core. In the eutrophic part, mackinawite was positively identified and represented the dominant Fe(II) sulfide phase. This finding agreed with chemical extraction, which indicated that18–40 mol% of Fe was contained in the acid volatile iron sulfide fraction. EXAFS spectra of the eutrophic section were best fitted by considering the admixture of mackinawite and the Fe–Ca carbonate phase inferred to be predominant in the oligotrophic regime.  相似文献   
7.
The speciation and thermodynamic properties of ferric chloride complexes in hydrothermal solutions and hypersaline brines are still poorly understood, despite the importance of this element as a micronutrient and ore-component. Available experimental data are limited to room temperature and relatively low chloride concentrations. This paper reports results of UV-Vis spectrophotometric and synchrotron XAFS experiments of ferric chloride complexes in chloride concentrations up to 15 m and at temperatures of 25-90 °C. Qualitative interpretation of the UV-Vis spectra shows that FeCl2+, FeCl2+, FeCl3(aq) and FeCl4 were present in the experimental solutions. As chloride concentrations increase, higher ligand number complexes become important with FeCl4 predominating in solutions containing more than 10 m at 25 °C. The predominance fields of FeCl3(aq) and FeCl4 expand to lower Cl concentrations with increasing T. Both XANES and UV-Vis spectra reveal a major change in the geometry of the complex between FeCl2+ and FeCl3(aq). EXAFS data confirm that the number of chloride ligands increases with increasing chloride concentration and show that Fe3+, FeCl2+ and FeCl2+ share an octahedral geometry. FeCl3(aq) could be either tetrahedral or trigonal dipyramidal, while FeCl4 is expected to be tetrahedral. EXAFS data support a tetrahedral geometry for FeCl4, especially at 90 °C, but do not allow to distinguish between a tetrahedral or trigonal dipyramidal geometry for FeCl3(aq) because of similar Fe-Cl distances. At room temperature, EXAFS data suggest that FeCl3(aq) may be a mixture of octahedral and tetrahedral or trigonal dipyramidal forms.The room temperature formation constants for three ferric chloride complexes (FeCl2+, FeCl3(aq) and FeCl4) determined from the UV data are generally in good agreement with previous studies. Calculations based on the properties extrapolated to 300 °C show that hematite solubility is much higher than previously estimated, and that the high orders complexes FeCl3(aq) and FeCl4 are important at high temperatures even in solutions with low chloride concentrations. The accuracy of these properties is limited by a poor understanding of activity-composition relationships in concentrated electrolytes, and by limitations in the available experimental techniques and extrapolation algorithms; however, the inclusion of higher order complexes in numerical models of ore transport and deposition allows for a more accurate qualitative prediction of Fe behaviour in hydrothermal and hypersaline systems.  相似文献   
8.
This paper presents the microstructural and structural properties of two natural salt samples from Iran and Portugal. Their strength-ductility behavior is explored by uniaxial compression experiments that, demonstrate that the observed differences lie not only in the inhomogeneous composition of the samples and their different grain sizes but also in their internal microstructural inhomogeneities. Microstructural inhomogeneities and substructural changes were observed with the SEM method (Scanning Electron Microscopy), the thin section microscope investigations and the EXAFS (Extended X-ray Absorption Fine Structure) spectroscopy. EBSD (Electron backscattered diffraction) analyses show maximum in the [100] or [110] directions in the inverse pole figure. This demonstrates that recrystallization and grain growth processes took place together. A weak [111] texture sometimes observed nearby indicates that residual stress is still present in the recrystallized sample.Comparison of the textural and structural results show that local structural rearrangements take place during textural development; this is attributed to different orientations influencing the deformation and recrystallization of adjacent grains influencing the bulk final texture.  相似文献   
9.
Natural ferrihydrites (Fh) often contain impurities such as aluminum, especially in acid mine drainage, and these impurities can potentially impact the chemical reactivity of Fh with respect to metal (loid) adsorption. In the present study, we have investigated the influence of aluminum on the sorption properties of ferrihydrite with respect to environmentally relevant aqueous arsenic species, arsenite and arsenate. We have conducted sorption experiments by reacting aqueous As(III) and As(V) with synthetic Al-free and Al-bearing ferrihydrite at pH 6.5. Our results reveal that, when increasing the Al:Fe molar ratio in Fh, the sorption density dramatically decreased for As(III), whereas it increased for As(V). Extended X-ray Absorption Fine Structure (EXAFS) spectroscopy analysis at the As K-edge indicated that the AsIIIO3 pyramid binds to FeO6 octahedra on both Al-free Fh and Al-bearing Fh, by forming bidentate mononuclear edge-sharing (2E) and bidentate binuclear corner-sharing (2C) surface complexes characterized by As–Fe distances of 2.9 Å and 3.4 Å, respectively. The decrease in As(III) sorption density with increasing Al:Fe ratio in Fh could thus be explained by a low affinity of the As(OH)3 molecule for Al surface sites compared to Fe ones. In contrast, on the basis of available literature on As(V) adsorption mechanisms, we suggest that, in addition to inner-sphere 2C arsenate surface complexes, outer-sphere arsenate surface complexes forming hydrogen bonds with both Al–OH and Fe–OH surface sites could explain the enhancement of As(V) sorption onto aluminous Fh relative to Al-free Fh, as observed in the present study. The presence of aluminum in Fh may thus enhance the mobility of arsenite with respect to arsenate in Acid Mine Drainage impacted systems, while mixed Al:Fe systems could present an alternative for arsenic removal from impacted waters, provided that As(III) would be oxidized to As(V).  相似文献   
10.
Experimentally, a feasibility study for adsorption and catalytic pyrolysis of spill oils on Cu/ZSM-5 for recycling of light oils has been conducted in the present work. The adsorption and pyrolysis of model compounds such as heptane, toluene, and diesel (to stimulate the spill oils) on Cu/ZSM-5 have been investigated on a continuous fixed-bed reactor. By component fitted X-ray absorption near edge structural (XANES) spectroscopy, catalytic active species such as metallic copper (Cu) (77-84%) and Cu(2)O (6-7%) are found in the channels of ZSM-5 during pyrolysis of heptane or toluene. Pyrolysis of diesel effected by Cu/ZSM-5 yields gas (C(1)-C(5)) (32%) and light oil (68%) that can be used as auxiliary fuels.  相似文献   
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