SPHERICAL GRATING MONOCHROMATOR (SGM) BEAMLINE

News/Highlights

Research Highlights
Mg K-edge XANES and EXAFS
Aug. 2, 2023
Dental enamel is a principal component of teeth, and has evolved to bear large chewing forces, resist mechanical fatigue and withstand wear over decades. Functional impairment and loss of dental enamel, caused by developmental defects or tooth decay (caries), affect human health and quality of life, with associated costs to society. Mg is an important component of dental enamel, hence, Mg molecular and atomic structural information can provide valuable information for understanding tooth development and decay.The position and intensity of transitions in Mg K-edge X-ray absorption near-edge structure (XANES) spectra are sensitive to the coordination number, geometry, bond length, and order at intermediate range. Many Mg-containing minerals can be identified by their spectral fingerprints. Spectra of rodent enamel lack the pre-A, D and E features that are characteristic for crystalline dolomite, huntite, and whitlockite. In contrast, the Mg-rich intergranular phase in rodent incisors shows a striking similarity to spectrum of synthetic Mg-substituted amorphous calcium phosphate (Mg-ACP). The dominant feature in the spectrum of synthetic Mg-ACP is the transition associated with the first coordination sphere (feature B), with little or no features that depend on order beyond the first shell. At the same time, the lower edge energy is indicative of a lower coordination number and shortrer Mg-O bond distance. The spectrum of human enamel is similar to those of rodent enamel or synthetic Mg-ACP yet display more pronounced A and B features. As these features are associated with electronic transitions in the first coordination and multiple scattering events from high shells, this indicates that a fraction of the Mg in human enamel is present in a crystalline rather than an amorphous environment, consistent with their incorporation into the crystalline core.The Mg K-edge extended X-ray absorption fine structure (EXAFS) of human enamel is nearly indistinguishable from that of rodent enamel or synthetic Mg-ACP. In sharp contrast to the crystalline reference compounds, in which numerous scattering features from more distant shells are apparent, spectra of enamel and synthetic Mg-ACP are dominated by the nearest neighbor shell. Analysis of the local environment around Mg by fitting EXAFS spectra with theoretical scattering paths reveals that the nerarest-neighbor Mg-O bond lengths in human enamel (2.09 A), rodent enamel (2.03 A) and synthetic Mg-ACP (2.02) are notably shorter than the Ca-O bonds in OHAp (2.40 A) and ACP (2.36 A). Unlike rodent enamel, where the Mg-O bond is shorter than the Mg-O bonds in the crystalline reference compounds (2.08 to 2.11 A), that of human enamel does fall into the range. In human and rodent enamel, and Mg-ACP, this shortening is accompanied by a reduction in the coordination number from 6 to ~4, which is indicative of an amorphous material and/or presence of water in the first coordination sphere. We conclude that the environment of the majority of Mg2+ in human enamel exhibits only short- to medium-range order, with a reduction in coordination number, and the possibility of water or hydroxyl ions in the first shell, similar to the environment of Ca in ACP. However, the Mg-O shortening is not as pronounced as in rodent enamel. This is consistent with a fraction of Mg2+ occupying distorted Ca(II) sites in the apatite lattice.DeRocher, Karen A., et al., 2020. Chemical gradients in human enamel crystallites. Nature 583: 66-71.
Research Highlights
Biocrusts in Forest Soils Stabilize OM
Sept. 1, 2021
Biological soil crusts (biocrusts) play an important role in the biogeochemical C-, N- and P-cycles but there is limited knowledge about their effect on the composition and stability of organic matter (OM) in soil. In pine and beech dominated temperate forests, the different compartments of biocrust, crust-adhering soil and crust-free soil were analysed by pyrolysis field ionization mass spectrometry (Py-FIMS) and C K-edge X-ray absorption near edge structure (XANES) spectroscopy. Phototrophic biocrust communities had been determined morphologically. Predominant tree species affected OM composition and stability but an overriding effect of biocrust organisms was observed. In biocrusts, the OM mineralization potential was high due to a high carbohydrate/ketone ratio and a high proportion of the fatty acid C22:0. A high proportion of free fatty acids in combination with a high carbohydrate proportion was identified as a relative marker for biocrusts and additional high proportions of lignin dimers were specific for samples under pine. In biocrust under pine, OM in soil compartments was characterized by large proportions of long-chain aliphatics from plant cuticular material. In A-horizon substrate under beech, OM compound classes were not affected by phototrophic species richness, suggesting functional redundancy of these biocrust organisms with regard to OM composition. In contrast to A-horizon substrate, OM in C-horizon substrate was characterized by a higher proportion of easily decomposable material. Under pine, forest management intensity (SMI) affected OM by stand age and density due to effects on phototrophic biocrust species. We conclude that compartment, vegetation, horizon substrate and SMI affected OM composition and stability, and biocrusts hence contributed to soil OM diversity in forest ecosystems.
Beamline Updates
Oct. 16, 2015
The final major component of the endstation, the detector array, is now installed.  Four silicon drift detectors are positioned 30 mm from the sample with a specific geometry that will provide multiple perspectives and optimize contrast.  3D printed caps are positioned over the detectors to prevent damage, reduce scattering background and hold thin film filters.
Beamline Updates
Sept. 17, 2015
Test measurements were made of a fly wing.  Images of a 2 x 2 mm field of view were acquired at a resolution of approximately 20 microns.  The lower image shows x-ray transmission and the upper image shows carbon fluorescence. An x-ray energy of 290 eV was used in the acquisition.
Beamline Updates
Aug. 13, 2015
The first x-ray images have been acquired on the SGM.  The test samples were a 0-80 nut and a gold mesh with a wire pitch of 20 microns.  A photon energy of 711 eV (Fe L-edge) was used and the total electron yield from the sample was used to generate the contrast in the images.
Beamline Updates
July 30, 2015
The KB mirrors have been successfully used to focus the beam to approximately 30 x 20 microns.  Optimization of the transmission and the beam demagnification will continue.
Beamline Updates
July 23, 2015
The two 150 mm long trapezoidal focusing mirrors were successfully installed on July 23rd.  Bending motors and encoders have been tested.
Beamline Updates
June 14, 2015
Testing of the KB mirror bender mechanism and motors is underway.  This system is 375 mm upstream from the sample and will focus the beam to 10 by 10 microns.
Beamline Updates
May 12, 2015
The vacuum compatible hexapod sample positioner has been installed and tested in the ambient pressure endstation.
Beamline Updates
May 9, 2015
Most of the parts have arrived and the construction of the new ambient pressure endstation has begun.