Nontronite is a significant component of commercially important nickel laterite ores. Its behavior during high-pressure acid leaching of such ores may have an impact upon the efficiency of the process. The present study was conducted in order to further investigate the response of this material during high-pressure acid leaching. In situ synchrotron powder X-ray diffraction data were collected from a number of nontronite samples during hydration and leaching reactions at ambient and elevated temperatures. The present study followed previous high-pressure acid-leaching studies of nontronite where unexpected contraction and expansion behavior of the clay was observed by means of in situ X-ray diffraction. In the earlier studies the data sets only extended to ~20 Å so that when the nontronite expanded to greater than 19.5 Å (hydrated) the main 001 peak was only partially visible in the observed d-spacing range. The aim of the current work was to collect similar in situ diffraction data over a greater d-spacing range to observe more fully the movement of the main 001 reflection in order to better understand the changes taking place. This work was undertaken at the powder diffraction beamline of the Australian Synchrotron which was configured such that an upper d-spacing limit of ~34.5 Å could be achieved. Suggestions arising out of the previous work were confirmed along with additional information from testing of samples from the Source Clays Repository of The ClayMinerals Society. These results also show contradictory behavior of clays with the layer charge distributed over tetrahedral and octahedral sheets.

The Royal Tyrrell Museum in Alberta, Canada is focused on reconstructing the communities that existed at the end of the Cretaceous. This challenge is made more difficult because for many of the taxa present, few complete specimens are preserved. In most smaller animals, all that remains preserved are isolated elements such as jaws. Teleost fish are of particular interest because they are dominant in today's aquatic communities. They are thought to have diversified after the Cretacious-Paleogene (K-Pg) mass extinction event, but many questions about early freshwater members of this group remain. Even the number of species present remains a mystery. Through an ambitious SR-μCT study we are non-destructively digitally dissecting both isolated elements and articulated skeletons that remain embedded in their rock matrix. Through comparison studies we are identifying features to aid in their identification while preserving the original fossils in an unaltered state for future studies.

Galeaclolusite, [Al6(AsO4)3(OH)9(H2O)4]⋅8H2O, is a new secondary hydrated aluminium arsenate mineral from Cap Garonne, Var, France. It forms crusts and spheroids of white fibres up to 50 μm long by 0.4 μm wide and only 0.1 μm thick. The fibres are elongated along [001] and flattened on (100). The calculated density is 2.27 g⋅cm–3. Optically, galeaclolusite is biaxial with α = 1.550(5), β not determined, γ = 1.570(5) (white light) and partial orientation: Z = c (fibre axis). Electron microprobe analyses coupled with crystal structure refinement results gives an empirical formula based on 33 O atoms of Al5.72Si0.08As2.88O33H34.12. Galeaclolusite is orthorhombic, Pnma, with a = 19.855(4), b = 17.6933(11), c = 7.7799(5) Å, V = 2733.0(7) Å3 and Z = 4. The crystal structure of galeaclolusite was established from its close relationship to bulachite and refined using synchrotron powder X-ray diffraction data. It is based on heteropolyhedral layers, parallel to (100), of composition Al6(AsO4)3(OH)9(H2O)4 and with H-bonded H2O between the layers. The layers contain [001] spiral chains of edge-shared octahedra, decorated with corner-connected AsO4 tetrahedra, that are the same as in the mineral liskeardite.

Advanced imaging techniques are enhancing research capacity focussed on the developmental origins of adult health and disease (DOHaD) hypothesis, and consequently increasing awareness of future health risks across various subareas of DOHaD research themes. Understanding how these advanced imaging techniques in animal models and human population studies can be both additively and synergistically used alongside traditional techniques in DOHaD-focussed laboratories is therefore of great interest. Global experts in advanced imaging techniques congregated at the advanced imaging workshop at the 2019 DOHaD World Congress in Melbourne, Australia. This review summarizes the presentations of new imaging modalities and novel applications to DOHaD research and discussions had by DOHaD researchers that are currently utilizing advanced imaging techniques including MRI, hyperpolarized MRI, ultrasound, and synchrotron-based techniques to aid their DOHaD research focus.

In this work, a Ti–29Nb–13Ta–4.6Zr–xO Gum Metal with two significantly different oxygen levels (388 and 3570 ppm) was investigated during deformation. The alloys were compressed during in situ high-energy X-ray diffraction using three different strain rates, 10−4, 10−3, and 10−1 s−1, in order to evaluate their influence on phase stability and mechanical properties. The influence of oxygen on the deformation process was also studied. Deformation takes place by twinning, stress-induced, and reverse martensitic transformation and was observed, for some samples, a spinodal decomposition of the β-phase during elastic deformation. The mechanical properties were similar for the different rates employed when considering the same oxygen level. The alloy with a higher amount of oxygen, however, showed a substantial increase in mechanical strength, with a yield strength of around 680 MPa, which is more than three times higher than for the specimen with 388 ppm of oxygen.

The extremotolerant bacterium Deinococcus radiodurans is used as a model to explore the limits of life on Earth and beyond. In experiments performed in an ultra-high vacuum chamber with a vacuum ultraviolet (VUV) synchrotron beamline, this microorganism was exposed to conditions present on an extraterrestrial environment unprotected by an atmosphere, such as outside a spacecraft or on an asteroid, relevant in the context of planetary protection and panspermia hypothesis. Different methods were used to obtain the biologically relevant information from this investigation. Counting of colony forming units, the traditional approach for viability assessment, is limited to measuring the survival of the cells. For a more in-depth study of damage mechanisms at subcellular levels, specific molecular probes (propidium iodide and dihydrorhodamine 123) were applied and whole populations could be analysed, cell by cell, by flow cytometry. VUV radiation caused a substantial loss of viability, though only a fraction of the cells presented membrane damages even at the largest tested fluences. Additionally, intracellular oxidative stress was also detected upon exposure. These results point to significant VUV inactivating effects extending beyond the cells' outermost structures, in contrast to a more superficial role that could be expected due to the highly interacting nature of this radiation range. Nevertheless, it was observed that microscopic-level shading sufficed to allow the persistence of a small surviving subpopulation for the longer expositions. This study contributes to unveiling the response of biological systems under space conditions, assessing not just cell viability but also the mechanisms that lead to inactivation.

High-resolution synchrotron X-ray diffraction recorded on a collection of palygorskites with different chemical compositions (obtained by analytical electron microscopy) permits unambiguous correlation of the crystallographic parameters a (or a sin β if a monoclinic phase is considered) with the nature of the octahedral sheet, i.e. with both the number of octahedral positions that are occupied and the type of octahedral cation. No significant changes in the lattice parameters b and c are observed. The unit cell modification consists essentially of an expansion in a as the number of cations with larger ionic radii (Mg2+ and Fe3+) predominates over smaller cations (Al3+). A linear dependency of a (or a sin β) on the chemical composition of the octahedral sheet was obtained that can be used for classifying palygorskite into compositional groups, using only conventional diffraction data, without the need for chemical analyses.

Synchrotron X-ray diffraction (XRD) is a powerful technique to study in situ and in real-time the structural and kinetic processes of pressure-induced phase transformations. This paper presents the experimental set-up developed at beamline ID27 of the ESRF to perform time-resolved angle dispersive XRD in the Paris-Edinburgh cell. It provides a practical guide for the acquisition of isobaric-isothermal kinetic data and the construction of transformation-time plots. The interpretation of experimental data in terms of reaction mechanisms and transformation rates is supported by an overview of the kinetic theory of solid-solid transformations, with each step of data processing illustrated by experimental results of relevance to the geosciences. Reaction kinetics may be affected by several factors such as the sample microstructure, impurities or differential stress. Further high-pressure kinetic studies should investigate the influence of such processes, in order to acquire kinetic information more akin to natural or technological processes.

The impact of human activities on biogeochemical cycles in terrestrial environments is nowhere more apparent than in urban landscapes. Trace metals, collected on roadways and transported by storm water, may contaminate soils and sediments associated with storm water management systems. These systems will accumulate metals and associated sediments may reach toxic levels for terrestrial and aquatic organisms using the retention basins as habitat. The fate and bioavailability of these metals once deposited is poorly understood. Here we present results from a dose-response experiment that examines the application of synchrotron X-ray fluorescence methods (μ-SXRF) to test the hypothesis that earthworms will bio-accumulate Zn in a roadway-dust contaminated soil system providing a potential pathway for roadway contaminants into the terrestrial food web, and that the storage and distribution of Zn will change with the level of exposure reflecting the micronutrient status of Zn.

Lumbricus friendi was exposed to Zn-bearing roadway dust amended to a field soil at six target concentrations ranging from background levels (45 mg/kg Zn) to highly contaminated levels (460 mg/ kg Zn) designed to replicate the observed concentration range in storm-water retention basin soils. After a 30 day exposure, Zn storage in the intestine is positively correlated with dose and there is a change in the pattern of Zn storage within the intestine. This relationship is only clear when μ-SXRF Zn map data is coupled with a traditional toxicological approach, and suggests that the gut concentration in L. friendi is a better indicator of Zn bioaccumulation and storage than the total body burden.

The type specimen of peisleyite has been reinvestigated by a combination of scanning electron microscopy, electron probe microanalysis (EPMA) and synchrotron powder X-ray diffraction. Morphological investigation showed that mats of peisleyite crystals, individually <3 μm across, are intergrown with wavellite veinlets to form the white cryptocrystalline material that is typical of ‘peisleyite’. New EPMA data (mean of 12 analyses) gave the empirical formula of peisleyite as (Na1.69Ca0.18)Σ1.87(Al9.04Fe0.03)Σ9.07[(P6.28S1.38Si0.25)O4]Σ7.91(OH)6.66·27.73H2O, or ideally Na2Al9[(P,S)O4]8(OH)6·28H2O. The associated wavellite was found to be F-rich. Synchrotron powder data were indexed and refined and gave the following unit cell: P1̄, a = 9.280(19), b = 11.976(19), c = 13.250(18) Å, α = 91.3(1), β = 75.6(1), γ = 67.67(1)°, V = 1308(5) Å3 and Z = 4. These data are significantly different to those reported in the original description of peisleyite.

The equation of state of synthetic deuterated burtite, CaSn(OD)6, has been determined to 7.25 GPa at 298 K by synchrotron X-ray powder diffraction. Fitting to a third-order Birch-Murnaghan equation of state gives K0 = 44.7(9) GPa and K0′ = 5.3(4). A second-order fit gives K0 = 47.4(4) GPa. Within experimental error the two fits are indistinguishable over the pressure range studied. The decrease in the a parameter with pressure is smooth and no phase transitions were observed. Burtite is much more compressible (by a factor of three or four) than CaSnO3 and CdSnO3 perovskites, indicating that the absence of a cavity cation has a major effect upon the compressibility of the octahedral framework. Burtite is also markedly more compressible than the closely-related mineral stottite FeGe(OH)6 (K0 = 78 GPa). Their different compressibilities correlate with the relative compressibilities of stannate and germanate perovskites. Although different octahedral compressions are likely to be the primary reason for the different compressibilities of burtite and stottite, we also consider the possible secondary role of hydrogen-bonding topology in affecting the compressibilities of protonated octahedral frameworks. Burtite and stottite have different hydrogen-bonding topologies due to their different octahedral-tilt system. Burtite, space group Pn and tilt system a+a+a+, has a hydrogen-bonded network of linked four-membered rings of O-H…O linkages, whereas stottite, space group P42/n and tilt system a+a+c−, has <100> O-H…O crankshafts and isolated four-membered rings. These different hydrogen-bonded configurations lead to different bracing of the empty cavity sites by the O-H…O linkages and very different hydrogen-bonding connectivities in these two minerals that may also enhance the difference between their compressibilities.

Transmission X-ray diffraction is demonstrated as a new tool for examining daughter minerals within sub-micrometre-size fluid inclusions in fibrous diamond. In transmission geometry, the X-ray beam passes through the sample, interacting with a volume of material. Fibrous diamonds from Mbuji-Mayi. Democratic Republic of Congo; the Wawa area, Ontario, Canada; and the Panda kimberlite, Ekati Mine, Northwest Territories and the Jericho kimberlite, Nunavut, Canada were analysed using X-rays from a high-brilliance lab source and a synchrotron source. Daughter minerals present include the mica-group mineral celadonite, sylvite, halite, dolomite and other carbonates. This represents the first positive identification of halide minerals in fibrous diamond. Mineral inclusions such as forsteritic olivine and pyrope garnet were also found. Unexpectedly, daughter minerals were identified in only ten of the 38 diamonds analysed, despite their concentrations being greater than experimentally proven detection limits. The presence of significant amounts of amorphous or dissolved material appears unlikely, but cannot be ruled out. Alternatively, the results may indicate a wide variety of related daughter minerals, such that most phases fall below the detection limits. Transmission X-ray diffraction should be applied cautiously to the study of fibrous diamond, as it provides an incomplete account of the fluid-inclusion mineralogy.

Bariopharmacoalumite-Q2a2b2c, Ba0.5(Cu,ZnO)0.1H0.6[Al4(OH)4(As0.9Al0.1O4)3]·5.5H2O, from the south mine of the old copper mine at Cap Garonne, France, has a 2 × 2 × 2 I-centred tetragonal superstructure of the basic pharmacosiderite-type structure. Cell parameters are a = 15.405(2) Å and c = 15.553(3) Å. The structure was determined and refined in I 2m to R 1= 0.057 for 2697 reflections with I > 2σ(I), using synchrotron X-ray data on a twinned crystal. The origin of the superlattice cell doubling was determined to be due predominantly to the ordering of Ba atoms in half of the [0 0 1] channels, centred at (0, 0, 0) and (½, ½, 0). The other channels, centred at (½, 0, 0) and (0, ½, 0), were found to be occupied by corner-connected chains of Cu/Zn-centred square planar units.

We present Raman data for camerolaite, cyanotrichite and carbonatecyanotrichite, and using synchrotron single-crystal X-ray diffraction have solved the structure of camerolaite from the Tistoulet Mine, Padern, Aude Department, France. Camerolaite crystallizes in space group P1 with the unit-cell parameters: a = 6.3310(13) Å, b = 2.9130(6) Å, c = 10.727(2) Å, α = 93.77(3)°, β = 96.34(3)°, γ =79.03(3)º, V = 192.82(7) Å3 and Z = ⅓, with respect to the ideal formula from the refinement, Cu6Al3(OH)18(H2O)2[Sb(OH)6](SO4). The crystal structure was solved to R1 = 0.0890 for all 1875 observed reflections [Fo > 4σFo] and 0.0946 for all 2019 unique reflections. The P cell has been transformed into a C-centred cell that aids comparison with that of the structurally related khaidarkanite by aC = 2aP – bP, giving parameters a = 12.441(3), b = 2.9130(6), c = 10.727(2) Å, α = 93.77(3), β = 95.57(3), γ = 92.32(3)º and Z = ⅔ in C1. Edge-sharing octahedral ribbons Cu2Al(O,OH,H2O)8 form hydrogen-bonded layers || (001), as in khaidarkanite. The partially occupied interlayer Sb and S sites of the average structure are in octahedral and tetrahedral coordination by oxygen, respectively. They cannot be occupied simultaneously, which leads to regular alternation of [Sb(OH)6]– and SO42– groups in rods || y, resulting in local tripling of the periodicity along y for the Sb(OH)6–SO4 rods. Thus, camerolaite has a ‘host–guest’ structure in which an invariant host module (layers of Cu–Al ribbons) has embedded rod-like guest modules with a longer periodicity. Coupling between the phases of these rods is only short-range, resulting in diffuse X-ray scattering rather than sharp superstructure reflections. Similar disorder is known for parnauite, and is deduced for other members of the cyanotrichite group (cyanotrichite, carbonatecyanotrichite and khaidarkanite). Group members all share the Cu–Al ribbon module but have interlayer rods of different compositions and topologies; thus, they form a merotypic family. The low symmetry of the camerolaite average structure suggests other possibilities for structure variation in the group, which are discussed.

In this study, direct evidence for the formation of magnetite via a green rust intermediate is reported. The Fe(II) induced transformation of ferrihydrite, was quantified in situ and under O2-free conditions using synchrotron-based time-resolved energy dispersive X-ray diffraction. At pH 9 and Fe(II)/Fe(III) ratios of 0.5 and 1, rapid growth (6 min) of sulphate green rust and its subsequent transformation to magnetite was observed. Electron microscopy confirmed these results, showing the initial rapid formation of hexagonal sulphate green rust particles, followed by the corrosion of the green rust as magnetite growth occurred, indicating that the reaction proceeds via a dissolution-reprecipitation mechanism. At pH 7 and Fe(II)/Fe(III) ratio of 0.5, sulphate green rust was the stable phase, with no transformation to magnetite.

A multi-anvil press was combined with monochromatic synchrotron X-ray radiation to investigate the synthesis, at high-pressure high-temperature conditions, of a recoverable bulk sample of Fe4O5, from an initial magnetite, Fe3O4, sample. Angle-dispersive diffraction patterns show that magnetite firstly breaks down, into an assemblage of hematite (Fe2O3) + Fe4O5. By increasing temperature at constant load, hematite disappears progressively by either reduction or by melting, or a combination of both. In the final product only Fe4O5 remains and, in the absence of hematite, can be kept stable and be recovered at ambient conditions. Refinement of the diffraction patterns at standard conditions demonstrate that Fe4O5 has the Sr2Tl2O5-type-structure with space group Cmcm and a = 2.8964(2) Å, b = 9.8225(6) Åand c = 12.5808(7) Å. This structure-type and related members of a homologous series, offer the possibility that the general sequence of AB(2+n)X(4+n) chemistries could, under certain conditions, be extended to accommodate prevalent oxygen fugacity or, indeed, other ordered stoichiometries through extension of the c axis by the addition of FeO6 octahedral blocks. This structural series, as in other systems, offers possibilities of hosting charge-transfer, Jahn-Teller and other electronic phenomena − as well as supporting metric distortions. Each of these possibilities is highlighted through illustration and extension to related structure-types, most notably from those of the spinels, post-spinels and post-perovskites.

The equation of state of Fo90 hydrous ringwoodite has been measured using X-ray powder diffraction to 45 GPa at the GSECARS beam line at the Advanced Photon Source synchrotron at Argonne National Laboratory. The sample was synthesized at 1400°C and 20 GPa in the 5000 ton multi anvil press at Bayerisches Geoinstitut in Bayreuth. The sample has the formula Mg1.70Fe0.192+ Fe0.023+H0.13- Si1.00O4 as determined by electron microprobe, Fourier transform infrared and Mössbauer spectroscopies, and contains ~0.79% H2O by weight. Compression of the sample had been been measured previously to 11 GPa by single crystal X-ray diffraction. A third-order Birch-Murnaghan equation of state fit to all of the data gives V0 = 530.49±0.07 Å3, K0 = 174.6±2.7 GPa and K' = 6.2±0.6. The effect of 1% H incorporation in the structure on the bulk modulus is large and roughly equivalent to an increase in the temperature of ∼600°C at low pressure. The large value of K' indicates significant stiffening of the sample with pressure so that the effect of hydration decreases with pressure.

The high-pressure monazite – scheelite structure transition has been observed at P >4.57 GPa in CaSeO4 by synchrotron X-ray powder diffraction. It is a first-order transition with a 4.5% volume change and is severely hindered kinetically. Scheelite-type CaSeO4 remains to a maximum experimental pressure of 42.2 GPa and no (002) reflection, specifically indicative of a subgroup transition to a fergusonite-type structure, is observed. Scheelite-type CaSeO4 remains at ambient conditions, where the tetragonal unit cell has parameters of a = 5.04801(11) c = 11.6644(5) Å and V = 297.21(3) Å3 with Dcalc = 4.090 g cm–3. The diffraction pattern of the recovered material was refined in space group I41/a to Rp = 0.98%, wRp = 1.91%, GoF = 0.59, RFobs = 5.04%, wRFobs = 4.27%. The oxygen is located on the general 16f site at (0.2578(8) 0.3699(14) 0.5755(4)) and shares four identical bonds with Se (4a: ½ ½ ½) at 1.644(5) Å. The Ca (4b: 0, 0, ½) is eight-coordinated via O at 4 × 2.440(6) Å and 4 × 2.504(5) Å. This is further evidence of the dissimilarity of sulfate and selenate at high pressure and temperature conditions and the closer resemblance of the selenates to the orthophosphates, arsenates and vanadates, where this type of transition sequence has been described.