More than a century of non-ferrous metallurgical activities have had a severe impact on the natural environment leading, in most heavily contaminated sites, to a complete loss of the vegetation cover (that is, desert-like areas) or to the selection of metal-hyperaccumulator plant species. Identifying the chemical forms of toxic metals is of vital importance for a realistic assessment of the chemical risk posed by their presence in soils and selecting effective remedia- tion technologies. In this study, X-ray diffraction (XRD), X-ray texture goniom- etry, and powder and polarized extended X-ray absorption fine structure (EXAFS, P-EXAFS) have been used to investigate quantitatively the speciation of Zn in soils contaminated by three smelters from northern France and Belgium, and coupled synchrotron-based micro-X-ray radiation fluorescence (SXRF) and mi- cro-EXAFS (EXAFS) were also used for one of these soils. Of these techniques, the application of P-EXAFS and EXAFS to molecular environmental science was unprecedented, and we show that their complementarity greatly improves the sensitivity of powder EXAFS to identify the nature of metal-containing minerals in soils. Franklinite (ZnFe2O4), willemite (Zn2SiO4), hemimorphite (Zn4Si2O7(OH)2 ·H 2O), and Zn-containing magnetite ((Fe,Zn)Fe2O4) were identi- fied in dense soil fractions by XRD and powder EXAFS. These primary minerals originate from atmospheric fallout of Zn dusts emitted during the pyrometallurgi- cal smelting process, and they act as the main source of Zn in contaminated soils. In all soil samples, Zn released in solution during the weathering of these high-temperature minerals is taken up partly by phyllosilicates and, to a lesser extent, by Mn and Fe (oxyhydr) oxides. Zn-containing phyllosilicates were identi- fied by comparing powder EXAFS spectra to a library of model compounds and from the noteworthy angular dependence of EXAFS spectra collected on self- supporting films of clay soil fractions. Analysis of higher correlations in EXAFS spectra suggests that the local structure around Zn in phyllosilicates is trioctahe- dral. The phyllomanganate Zn-sorbed birnessite and Zn-containing Fe grains having a FeOOH-like local structure were unambiguously identified bySXRF— EXAFS. In birnessite Zn is sorbed in the interlayer space above/below vacant sites and can be either 4-fold or 6-fold coordinated depending, presumably, on the anionic stacking of birnessite layers. Based on this micro-mineralogical investiga- tion, a satisfactory fit of the three identified Zn species (that is, phyllosilicate, Mn, and Fe (oxyhydr)oxides) to experimental powder EXAFS spectra of all clay soil fractions was obtained. The significance, origin, and stability of Zn-phyllosilicates are discussed. Specifically, we show that the formation of Zn-containing phyllosili- cates is consistent with calculated thermodynamic solubilities. For the range of measured Zn 2 (D10 ppm), Si(OH)4 (10-20 ppm), and H (5.6 F pH F 7.5) concen- trations, soil solutions are supersaturated (pH G 6) or near saturation (pH F 6) with respect to the trioctahedral Zn phyllosilicate, Zn-kerolite. Finally, the plausi- bility of the formation of (Zn,Al) hydrotalcite-like species contemplated by Julliot (1999) is critically assessed.

Quantitative zn speciation in smelter-contaminated soils by exafs spectroscopy

http://xraysweb.lbl.gov/uxas/Publicatons/Papers/pdfs/strawn%20geoderma.pdf

Microscale investigation into the geochemistry of arsenic, selenium, and iron in soil developed in pyritic shale materials

We report the results of our research and development in techniques for producing elliptical x-ray mirrors by controlled bending of a flat substrate. We review the theory and technique of mirror bending with emphasis on the optical engineering issues and describe our design concepts for both metal and ceramic mirrors. We provide analysis of the various classes of error that must be addressed to obtain a high quality elliptical surface and a correspondingly fine focus of the x-ray beam. We describe particular mirrors that have been built, using these techniques, to meet the requirements of the scientific program at the Advanced Light Source at Lawrence Berkeley National Laboratory. For these examples, we show optical metrology results indicating the achievement of surface accuracy values around and, in some cases, below 1 mrad as well as x-ray measurements showing submicrometer focal spots. © 2000 Society of Photo-Optical Instrumentation Engineers. (S0091-3286(00)01410-0)

/pdf/theory-and-practice-of-elliptically-bent-x-ray-mirrors-n8hes98wex.pdf

Theory and practice of elliptically bent x-ray mirrors

Characterization of Conditions Required for X-Ray Diffraction Experiments with Protein Microcrystals

A new Kirkpatrick-Baez-type focusing mirror system for use in synchrotron radiation IR beamlines is designed and fabricated. This mirror system, which contains two fifth-order-polynomial-corrected cylindrical mirrors, can collect and focus the long arc shape IR source from the bending magnet into a nearly perfect point image. To fabricate these two uncommon mirrors, 17-4 PH type stainless steel substrates are chosen and mechanically bent from planar to the desired fifth-order-polynomial-corrected cylindrical shapes with central radii of 3.74 and 5.43 m. The root mean square (rms) roughness and the slope error of these two mirrors are measured to be 0.3 nm and less than 6.3 µrad, respectively. The method for calculating the polynomial coefficients of both mirrors as well as the mirror fabrication process, mechanical design, and the method for adjusting the mirror shape using a long trace profiler are presented.

/pdf/new-focusing-mirror-system-for-synchrotron-radiation-2djbqh3vsy.pdf

New focusing mirror system for synchrotron radiation infrared beamlines

Of the many methods used to focus x-rays, the use of mirrors with an elliptical curvature shows the most promise of providing a sub-micron white light focus. Our group has been developing the techniques of controlled bending of mirror substrates in order to produce the desired elliptical shape. We have been successful in producing surfaces with the required microradian slope error tolerances. Details of the bending techniques used, results from laboratory slope error measurements using a Long Trace Profiler (LTP) and data from the measurement of focus shape using knife edge and imaging methods using x-rays in the 5-12 KeV energy range are presented. The development of a white light focusing opens many possibilities in diffraction and spectroscopic studies.

/pdf/progress-towards-sub-micron-hard-x-ray-imaging-using-5a6vp0hnmt.pdf

Progress towards sub-micron hard x-ray imaging using elliptically bent mirrors

/pdf/progress-towards-sub-micron-hard-x-ray-imaging-using-2zidcapnp7.pdf

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Progress towards sub-micron hard x-ray imaging using elliptically bent mirrors

Progress towards sub-micron hard x-ray imaging using elliptically bent mirrors