Study of mineralogical speciation of arsenic in soils using X ray microfluorescence and scanning electronic microscopy

In this paper we studied the As content in natural contaminated soils, classified as Dystric Leptosol, Chromic Luvisol, Eutric Cambisol and Mollic Leptosol. In soil samples, sieved (<2 mm), total As was determined by XRF and chemical speciation by sequential extraction. As-bearing minerals were concentrated from fine sand fraction of soil (200-20 μm) using heavy liquid. In this fraction, mineralogical speciation was studied by X-ray microfluorescence, XRD with Göbbel mirror and SEM-BEI-EDX. Total As contents ranging from 61.00 to 131.00 mg kg⁻¹. The results of the sequential extraction showed that As was, mainly, in the residual fraction (52.51-98.76 mg kg⁻¹) and in the fraction bound to iron oxyhydroxides (0-36.5 mg kg⁻¹). Mapping of As with X-ray microfluorescence show strongly relationship between Fe and As. Iron (III) oxyhydroxides (FeOHs) (lepidocrocite and goethite), scorodite, angelellite, schultenite and dussertite were identified by XRD analysis as most likely mineral phases. The contents of As, Fe, Pb and Ba obtained with EDX-microprobe, confirmed the results of XRD. The results of sequential extraction and X-ray microfluorescence indicate that As is strongly bound to the soils because the identified As-bearing mineral phases are very stable at the pH conditions of studied soils. Consequently, a low mobility of As can be assumed in these soils.     

High‐flux hard X‐ray microbeam using a single‐bounce capillary with doubly focused undulator beam

A pre‐focused X‐ray beam at 12 keV and 9 keV has been used to illuminate a single‐bounce capillary in order to generate a high‐flux X‐ray microbeam. The BioCAT undulator X‐ray beamline 18ID at the Advanced Photon Source was used to generate the pre‐focused beam containing 1.2 × 10¹³ photons s^?1 using a sagittal‐focusing double‐crystal monochromator and a bimorph mirror. The capillary entrance was aligned with the focal point of the pre‐focused beam in order to accept the full flux of the undulator beam. Two alignment configurations were tested: (i) where the center of the capillary was aligned with the pre‐focused beam (`in‐line') and (ii) where one side of the capillary was aligned with the beam (`off‐line'). The latter arrangement delivered more flux (3.3 × 10¹² photons s^?1) and smaller spot sizes (≤10 µm FWHM in both directions) for a photon flux density of 4.2 × 10¹⁰ photons s^?1µm^?2. The combination of the beamline main optics with a large‐working‐distance (approximately 24 mm) capillary used in this experiment makes it suitable for many microprobe fluorescence applications that require a micrometer‐size X‐ray beam and high flux density. These features are advantageous for biological samples, where typical metal concentrations are in the range of a few ng cm^?2. Micro‐XANES experiments are also feasible using this combined optical arrangement.     

用XRMF分段多项式回归法定量分析铂钯合金

在Ｘ射线荧光分析中,当工体效应严重时,工作曲线变得很复杂,仅用一条曲线来拟合,误差较大,为此,采用的分段的方法,将工作曲线分成四段,逐段拟合,取得了很好的效果。拟合工作曲线时,所使用的铂钯合金标样,由Ｘ射线微探针（ＸＲＭＦ）测试。此外,我们还用这种方法,分析了标样薄片中元素分布的均匀性水平。     

TiO2 distribution in aged and injected isotactic polypropylene parts by synchrotron radiation X‐ray microfluorescence

We studied the TiO₂ pigment distribution along cross sections of injected isotactic polypropylene samples after they were aged by light exposure for 515 and 3000 h in accelerated test equipment. The TiO₂ pigment distribution was studied so that we could understand the whitening process occurring in this type of plastic. For these studies, we used a 20‐μm X‐ray microbeam from a synchrotron light source. We observed that the aged and nonaged samples had almost homogeneous distributions of Ti in the cross sections; therefore, pigment migration could not have been responsible for the surface whitening process. There were maxima of Ti intensities that were not in the same region for all samples. This behavior could be explained by the heterogeneity of the extrusion and injection‐molding processes. © 2002 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 40: 657–662, 2002; DOI 10.1002/polb.10127