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At least 19 records

Three Dimensional Structures of Particles Recovered from the Asteroid Itokawa by the Hayabusa Mission and a Role of X-Ray Microtomography in the Preliminary Examination

Particles of regolith on S-type Asteroid 25143 Itokawa were successfully recovered by the Hayabusa mission of JAXA (Japan Aerospace Exploration Agency). Near-infrared spectral study of Itokawa s surface indicates that these particles are materials similar to LL5 or LL6 chondrites. High-resolution images of Itokawa's surface suggest that they may be breccias and some impact products. At least more than 1500 particles were identified as Itokawa origin at curation facility of JAXA. Preliminary analysis with SEM/EDX at the curation facility shows that they are roughly similar to LL chondrites. Although most of them are less than 10 micron in size, some larger particles of about 100 micron or larger were also identified. A part of the sample (probably several tens particles) will be selected by Hayabusa sample curation team, and sequential examination will start from January 2011 by Hayabusa Asteroidal Sample Preliminary Examination Team (HASPET). In mainstream of the analytical flow, each particle will be examined by microtomography, XRD and XRF first as nondestructive analyses, and then the particle will be cut by an ultra-microtome and examined by TEM, SEM, EPMA, SIMS, PEEM/XANES, and TOF-SIMS sequentially. Three-dimensional structures of Itokawa particles will be obtained by microtomography sub-team of HASPET. The results together with XRD and XRF will be used for design of later destructive analyses, such as determination of cutting direction and depth, to obtain as much information as possible from small particles. Scientific results and a role of the microtomography in the preliminary examination will be presented.

Tsuchiyama, A.↗

Characterizing the pore-scale impacts of enhanced-solubilization solutions on organic-liquid morphology and fluid-fluid interfacial area with microtomography

Synchrotron X-ray microtomography was used to directly quantify the impact of enhanced-solubilization solutions on mobilization of a non-wetting fluid in a natural porous medium. Polyoxyethylene sorbitan monooleate (tween 80), hydroxypropyl-β-cyclodextrin (HPCD), sodium dodecyl sulfate (SDS), and ethanol were used as the solubilization reagents. Tetrachloroethene (PCE) was used as the entrapped organic immiscible liquid. Microtomography images were collected prior to and after successive floods with each reagent solution. The total trapping number was varied by more than three orders of magnitude by changing the velocity and viscosity of the aqueous phase as well as the interfacial tension between fluid phases. The results were compared to those obtained from equivalent experiments conducted with water flooding. Inspection of images indicated that mobilization caused a change in PCE morphology and distribution for all reagents with the exception of HPCD, for which a lower trapping number was determined compared to the other experiments. Mobilization of organic liquid was observed at total trapping numbers that were consistent with prior work. The enhanced-solubilization solutions had minimal impact on the configuration or magnitude of fluid-fluid interfacial area.

Interfacial area↗

The metrology of spherical shells using synchrotron x ray microtomography

With recent advances in solid state imaging technology and the increasing availability of synchrotron x-ray radiation sources, synchrotron x-ray microtomography is emerging as a nondestructive technique for the evaluation of the structure and composition of small specimens with spatial resolution in the micron range. Synchrotron radiation offers the following advantages over conventional x-ray sources: high brightness, continuous emission which is tunable over a large energy range, faster data collection rates, and a highly collimated beam of large cross section permitting the illumination of large specimens. Synchrotron x-ray microtomography enables the structure of individual spheres to be evaluated in order to reveal the concentricity and sphericity of the internal void and the uniformity of the shell wall in the case of high quality spherical shells for Sandia National Laboratories' Inertial Confinement Fusion project.

Hmelo, Anthony B.↗

Reduced volume of diabetic pancreatic islets in rodents detected by synchrotron X-ray phase-contrast microtomography and deep learning network

The pancreatic islet is a highly structured micro-organ that produces insulin in response to rising blood glucose. Here we develop a label-free and automatic imaging approach to visualize the islets in situ in diabetic rodents by the synchrotron radiation X-ray phase-contrast microtomography (SRμCT) at the ID17 station of the European Synchrotron Radiation Facility. The large-size images (3.2 mm × 15.97 mm) were acquired in the pancreas in STZ-treated mice and diabetic GK rats. Each pancreas was dissected by 3000 reconstructed images. The image datasets were further analysed by a self-developed deep learning method, AA-Net. All islets in the pancreas were segmented and visualized by the three-dimension (3D) reconstruction. After quantifying the volumes of the islets, we found that the number of larger islets (=>1500 μm 3 ) was reduced by 2-fold (wt 1004 ± 94 vs GK 419 ± 122, P < 0.001) in chronically developed diabetic GK rat, while in STZ-treated diabetic mouse the large islets were decreased by half (189 ± 33 vs 90 ± 29, P < 0.001) compared to the untreated mice. Our study provides a label-free tool for detecting and quantifying pancreatic islets in situ. It implies the possibility of monitoring the state of pancreatic islets in vivo diabetes without labelling.

59 BASIC BIOLOGICAL SCIENCES↗

X-Ray Microtomography Measurements of Coevolving Particle Size and Shape

This study measures simultaneous changes in particle size and shape during grain crushing and proposes quantitative metrics to track their coevolving statistical distribution. Idealized granular materials with widely different initial particle shapes (i.e., spheres, quasi-ellipsoids, plates, and rods) are compressed oedometrically at vertical stress levels sufficient to induce particle breakage. X-ray microtomography and digital image analysis are then used to track changes in particle-scale characteristics. The observations indicate that more irregular particles tend to exhibit a higher degree of breakage compared to more spherical grains subjected to an equivalent stress level. Despite these differences, the measurements also indicate that all the tested particle sets approach a common attractor (expressed in terms of aspect ratio, flatness, and elongation), regardless of their initial morphology. A new shape evolution index is proposed to quantify such trends. With this new metric, it is shown that in all the tested materials, the particle shape evolves faster than size, especially for the more regular morphologies, thus implying that the shape tends to reach its attractor point before the grading reaches its ultimate particle size distribution. Furthermore, this finding underpins an ultimate stage of crushing-driven compression that occurs with particle size reduction but minimal shape changes (i.e., self-replicating shapes due to fractures).

Oedometric compression↗

Focused‐beam X‐ray fluorescence and diffraction microtomographies for mineralogical and chemical characterization of unsectioned extraterrestrial samples

Abstract This study describes the application of new synchrotron X‐ray fluorescence (XRF) and diffraction (XRD) microtomographies for the 3‐D visualization of chemical and mineralogical variations in unsectioned extraterrestrial samples. These improved methods have been applied to three compositionally diverse chondritic meteorite samples that were between 300 and 400 μm in diameter, including samples prepared from fragments of the CR2 chondrite LaPaz Icefield (LAP) 02342, H5 chondrite MacAlpine Hills (MAC) 88203, and the CM2 chondrite Murchison. The synchrotron‐based XRF and XRD tomographies used are focused‐beam techniques that measure the intensities of fluorescent and diffracted X‐rays in a sample simultaneously during irradiation by a high‐energy microfocused incident X‐ray beam. Measured sinograms of the emitted and diffracted intensities were then tomographically reconstructed to generate 2‐D slices of XRF and XRD intensity through the sample, with reconstructed pixel resolution of 1–2 μm, defined by the resolution of the focused incident X‐ray beam. For sample LAP 02342, primary mineral phases that were visualized in reconstructed slices using these techniques included isolated grains of α‐Fe, orthopyroxene, and olivine. For our sample of MAC 88203, XRF/XRD tomography allowed visualization of forsteritic olivine as a primary mineral phase, a vitrified fusion crust at the sample surface, identification of localized Cr‐rich spinels at spatial resolutions of several micrometers, and imaging of a plagioclase‐rich glassy matrix. In the sample of Murchison, major identifiable phases include clinoenstatite‐ and olivine‐rich chondrules, variable serpentine matrix minerals and small Cr‐rich spinels. Most notable in the tomographic analysis of Murchison is the ability to quantitatively distinguish and visualize the complex mixture of serpentine‐group minerals and associated tochilinite–cronstedtite intergrowths. These methods provide new opportunities for spatially resolved characterization of sample texture, mineralogy, crystal structure, and chemical state in unsectioned samples. This provides researchers an ability to characterize such samples internally with minimal disruption of sample micro‐structures and chemistry, possibly without the need for sample extraction from some types of sampling and capture media.

Geochemistry & Geophysics↗

Using Low-Field Nuclear Magnetic Resonance and X-Ray Computed Microtomography Imaging to Explore Potential of Microbially-Induced Calcium Carbonate Precipitation Treatment to Seal Shale Fractures

Microbially-induced calcium carbonate precipitation (MICP) is a biological process in which microbially produced urease enzymes convert urea and calcium into solid calcium carbonate (CaCO 3 ) deposits. Studies have shown that MICP can be used to seal fractures in shale, raising the possibility of applying this technology to restimulate fracking wells by plugging underperforming fractures. For this and other applications to become a reality, non-invasive tools are needed to determine how effectively MICP seals shale fractures under subsurface conditions. In this study, a 2.54 cm wide and 5.08 cm long Marcellus shale core with a single, ~1 mm wide fracture held open by sand "proppant" underwent MICP-treatment at 60°C until reaching three orders of magnitude permeability reduction. Low-field nuclear magnetic resonance (LF-NMR) and X-Ray computed microtomography (μ-CT) techniques were used to assess the extent of biomineralization within the fracture. These tools revealed that while CaCO 3 precipitation occurred throughout the fracture, there was preferential precipitation around proppant, and the core sealed at the effluent end before filling most of the fracture. Both tools were able to independently calculate of the amount of solid biomineral formed inside the fracture. Furthermore, this study found that the distribution of proppant within the shale fracture was an important parameter controlling the degree of biomineralization.

clastic rock↗

Search for Organic Nanoglobules in Carbonaceous Chondrites Using Microtomography

Primitive solar materials have various organic matters. In recent years, novel organic materials called organic nanoglobules of a few hundred micrometers in typical size were discovered in carbonaceous chondrites, IDPs, and comet 81P/Wild 2. The organic globules are spherical shape and in many cases with hollow structures. Composition of the globules are mainly aromatic carbon. The isotopic anomalies of SD and 6N 15 observed in the globules indicate that they were formed from photochemical reaction to ice particles at very low temperature environment, such as molecular clouds or outer protosolar disk. Aqueous alteration of organic matters and the gamma-ray irradiation to PAH are also suggested as alternative possible formation processes. If the globules are made from organic ice particles, the hollow regions of the globules are suggested to be once filled with volatile H20-rich organic ices, while if they were formed by aqueous alteration, the hollow regions should be filled with a fluid which caused the aqueous alteration. However, fluids in the globules have not been detected so far in the previous studies. If fluids were originally preserved in the hollows, they might be lost during destructive processes of sample separation or preparation for TEM observation. X-ray computed tomography (CT) is a nondestructive method which can determine 3-D internal structures of objects. SR (synchrotron radiation)-based imaging microtomography can give submicron spatial resolution [8] and was applied to micro textures in extraterrestrial materials, such as cometary grains captured by the Stardust mission [9]. If organic globules are observed non-destructively in carbonaceous chondrites by tomography, we can check the presence of fluids in the hollows. If fluids are preserved, we may analyze chemical and isotopic compositions of the fluids. The purpose of this study is to observe organic nanoglobules using imaging tomography for future analysis.

Matsumoto, T.↗

Effect of Tube-Based X-Ray Microtomography Imaging on the Amino Acid and Amine Content of the Murchison CM2 Chondrite

X-ray and synchrotron X-ray micro-computed tomography (micro-CT) are increasingly being used for three dimensional reconnaissance imaging of chondrites and returned extraterrestrial material prior to detailed chemical and mineralogical analyses. Although micro-CT imaging is generally considered to be a non-destructive technique since silicate and metallic minerals in chondrites are not affected by X-ray exposures at the intensities and wavelengths typically used, there are concerns that the use of micro-CT could be detrimental to the organics in carbonaceous chondrites. We recently conducted a synchrotron micro-CT experiment on a powdered sample of the Murchison CM2 carbonaceous chondrite exposed to a monochromatic high energy (approximately 48 kiloelectronvolts) total X-ray radiation dose of approximately 1 kilogray (kGy) using the Advanced Photon Source beamline 13-BMD (13-Bending Magnet-D Beamline) at Argonne National Laboratory and found that there were no detectable changes in the amino acid abundances or enantiomeric compositions in the chondrite after exposure relative to a Murchison control sample that was not exposed. However, lower energy bremsstrahlung X-rays could interact more with amino acids and other lower molecular weight amines in meteorites. To test for this possibility, three separate micro-CT imaging experiments of the Murchison meteorite using the GE Phoenix v/tome/x s 240 kilovolt microfocus high resolution tungsten target X-ray tube instrument at the American Museum of Natural History (AMNH) were conducted and the amino acid abundances and enantiomeric compositions were determined. We also investigated the abundances of the C1-C5 amines in Murchison which were not analyzed in the first study.

Microtomography Imaging↗

Effect of a Synchrotron X-ray Microtomography Imaging Experiment on the Amino Acid Content of a CM Chondrite

X-ray microcomputed tomography and synchrotron X-ray microcomputed tomography (μCT) are becoming popular tools for the reconnaissance imaging of chondrites. However, there are occasional concerns that the use of μCT may be detrimental to organic components of a chondrite. Soluble organic compounds represent ~2–10% of the total solvent extractable carbon in CI and CM carbonaceous chondrites and amino acids are among the most abundant compounds in the soluble organic fraction. We irradiated two samples of the Murchison CM2 carbonaceous chondrite under conditions slightly harsher (increased beam exposure time) than those typically used for x-ray μCT imaging experiments to determine if detectable changes in the amino acid abundance and distribution relative to a nonexposed control sample occurred. After subjecting two meteorite portions to ionizing radiation dosages of 1.1 kiloGray (kGy) and 1.2 kGy with 48.6 and 46.6 keV monochromatic X-rays, respectively, we analyzed the amino acid content of each sample. Within analytical errors, we found no differences in the amino acid abundances or enantiomeric ratios when comparing the control samples (nonexposed Murchison) and the irradiated samples. We show with calculations that any sample heating due to x-ray exposure is negligible. We conclude that a monochromatic synchrotron X-ray μCT experiment at beamline 13-BM-D of the Advanced Photon Source, which imparts ~1 kGy doses, has no detectable effect on the amino acid content of a carbonaceous chondrite. These results are important for the initial reconnaissance of returned samples from the OSIRIS-REx and Hayabusa 2 asteroid sample return missions.

Jon M. Friedrich↗

Effect of 16-Day Spaceflight on the Morphology of Thick-Toed Geckos (Pachydactylus Bibronii Smith, 1846)

There are grounds to believe that space flown experiments on thick-toed geckos may help solve the problem of floatation of vertebrates in microgravity. Geckos of this species carry on the lower surface of their toes numerous setae, which allow them to remain attached to any surfaces regardless of the gravitational effects. Experiments were performed on 5 animals in each of the following groups: flight, basal, synchronous and laboratory controls. 32 hours after a 16- day flight the animals were euthanazed and examined using traditional histology and X-ray microtomography. Body mass losses were 10% in the flight animals, 7.4% in the synchronous controls, and 12.3% in the laboratory controls. Since the flight and synchronous animals were kept at 15-19 C, whereas the laboratory controls - at 26-28 C, it can be inferred that environmental temperatures impacted animal metabolism no less than flight induced stress. Blood tests of the flown animals showed a 12% decrease of erythrocytes and a 40% decrease of dark-nuclear granulocytes, with the number of light-nuclear granulocytes remaining unchanged. In the small intestine the number of goblet cells increased allowing them to occupy a large portion of the cyptal surface. Enhanced secretion was accompanied by the appearance of dead intestinal cells in the lumen. Clusters of degraded hepatocytes were found at the liver edges of flight animals. Signs of liver involution were similar to the changes produced by alcohol consumption but did not spread to its central part. In the heart, insignificant hypertrophy and excessive blood supply that still remained within the physiological norm were detected. No significant changes were found in the pancreas, lungs, nervous systems or the snouts of the flown animals, but the volume of their gallbladders was greater than in controls. The epithelium of toe pads of the flight animals became thinner. Histological examination of the humerus did not demonstrate significant mineral losses. However, X-ray microtomography showed changes in the trabecular structure in the subepyphyseal zone of bones in flight animals compared to the controls. In summary, all the changes detected in the flight animals were adaptive. Therefore, geckos of this species can be used as an animal model for morphological studies in longer-duration space flights.

Gulimova, V. I.↗

Search for Fluid Inclusions in a Carbonaceous Chondrite Using a New X-Ray Micro-Tomography Technique Combined with FIB Sampling

Early solar system aqueous fluids are preserved in some H chondrites as aqueous fluid inclusions in halite (e.g., [1]). Although potential fluid inclusions are also expected in carbonaceous chondrites [2], they have not been surely confirmed. In order to search for these fluid inclusions, we have developped a new X-ray micro-tomography technique combined with FIB sampling and applied this techniqu to a carbanaceous chondrite. Experimental: A polished thin section of Sutter's Mill meteorite (CM) was observed with an optical microscope and FE-SEM (JEOL 7001F) for chosing mineral grains of carbonates (mainly calcite) and sulfides (FeS and ZnS) 20-50 microns in typical size, which may have aqueous fluid inclusions. Then, a "house" similar to a cube with a roof (20-30 microns in size) is sampled from the mineral grain by using FIB (FEI Quanta 200 3DS). Then, the house was atached to a thin W-needle by FIB and imaged by a SR-based imaging microtomography system with a Fresnel zone plate at beamline BL47XU, SPring-8, Japan. One sample was imaged at two X-ray energies, 7 and 8 keV, to identify mineral phases (dual-enegy microtomography: [3]). The size of voxel (pixel in 3D) was 50-80 nm, which gave the effective spatial resolution of approx. 200 nm. A terrestrial quartz sample with an aqueous fluid inclusion with a bubble was also examined as a test sample by the same method. Results and discussion: A fluid inclusion of 5-8 microns in quartz was clearly identified in a CT image. A bubble of approx. 4 microns was also identified as refraction contrast although the X-ray absorption difference between fluid and bubble is small. Volumes of the fluid and bubble were obtained from the 3D CT images. Fourteen grains of calcite, two grains of iron sulfide and one grain of (Zn,Fe)S were examined. Ten calcite, one iron sulfide and one (Zn,Fe)S grains have inclusions >1 micron in size (the maximum: approx. 5 microns). The shapes are spherical or irregular. Tiny inclusions (<1 micron) are also present in all the grains examined. These results show that mineral grains have more inclusions than expected from 2D observations. The X-ray absorption of the inclusions shows that they are not solid inclusions. No bubbles were observed inside, indicating that we cannot determine whether they are really aqueous fluids or merely voids. One calcite grain has an inclusion approx. 2 microns in size, which seems to have a bubble and a tiny solid daughter crystal inside (three-phase inclusion). As we know the exact 3D position of the inclusion, we will anlyze the inclusion by SIMS after freezing the sample as has been done for a halite sample [3]. The present technique is useful for finding small inclusions not only in carbonaceous chondrites but also for terrestrial materials.

Tsuchiyama, A.↗

Additive manufacturing of mullite ceramic by digital light processing

Mullite material was successfully additively manufactured using digital light processing (DLP). The printed geometry involves a one-step process of pyrolysis, de-binding, and sintering under a plain atmosphere to achieve an average of 76 % ceramic yield and linear shrinkage of 12 %. Furthermore, the thermal profile was carefully controlled to obtain consistent phases in which the XRD shows a mullite phase. Here, in addition, the Weibull analysis was conducted on the sintered flexural specimens, showing a Weibull modulus (m) of 13.05 with a characteristic strength (σ 0 ) of 94.96 MPa. Synchrotron microtomography was performed on the sintered specimens, which showed two distinct porosity distributions (small and large). Large porosity (non-spherical elongated) is the primary cause of decreased material strength, while small porosity (spherical) is the sintering product. The measured thermal conductivity of the specimens was in the range of 2.7–3.1 W/m∙k and decreased with an increase in temperature. Lastly, large-scale prototypes were printed concurrently with a fine resolution of 25 μm without any compromise on the predetermined design and structure.

Additive manufacturing↗

Strong effect of liquid Fe–S on elastic wave velocity of olivine aggregate: Implication for the low velocity anomaly at the base of the lunar mantle

The origin of the seismic low velocity zone (LVZ) observed at the base of the lunar mantle is important for understanding the nature of the lunar mantle. Liquid Fe–S is considered as a possible candidate of the cause of the LVZ. However, effect of liquid Fe–S on elastic wave velocity of mantle rock has been considered to be minor, according to theoretical estimation based on the high dihedral angle of liquid Fe–S in olivine aggregate observed in previous microstructural analysis of polished sample cross sections. Here, in this work, we carry out direct measurements of elastic wave velocities of liquid Fe–S-bearing olivine aggregate and report strong reduction of the elastic wave velocities in the presence of liquid Fe–S. The effects of liquid Fe–S in olivine aggregates are much more pronounced than the theoretical estimation. Three-dimensional X-ray microtomography analysis reveals that the geometry of liquid Fe–S strongly depends on the size, with larger liquid Fe–S blobs having low aspect ratios, which may predominantly affect elastic wave velocity. Since smaller spherical Fe–S blobs are much more abundant than the larger elongated blobs, conventional dihedral angle analyses based on scanning electron microscope images tend to statistically over-sample smaller blobs and under-sample larger blobs. Our results suggest that the LVZ at the base of the lunar mantle can be explained by the presence of 4.3–5.0 vol.% liquid Fe–S. The LVZ may be a hidden reservoir of highly siderophile elements (HSEs), which may explain the low abundance of HSEs in the lunar mantle compared to the Earth.

58 GEOSCIENCES↗

Dissolution and reprecipitation of amorphous silica in silica Rich shales induces Non-Monotonic evolution of porosity in acidic reactive environments

Advances in sustainable subsurface energy technologies are crucial for meeting our energy and resource needs for a climate-resilient future. Novel strategies to harness subsurface shale reservoirs for recovering valuable metals and for enabling CO 2 storage are influenced by the morphological and mineralogical heterogeneities of these materials. In this context, delineating the interactions of highly acidic solutions such as wet supercritical CO 2 on shales with varying mineralogy is crucial to inform the stability of caprock seal for CO 2 storage and enhancements in permeability for fluid transport, reactivity, and storage. The feedback chemical effects associated with the interactions of acidic solutions on the morphologies and mineralogies of shales have not been extensively investigated. These insights are crucial for assessing temporal changes in the reactivity and the fate of the fluids in subsurface environments. In this study, we investigate the effect of 1M HCl solution on the chemistry and morphology of three different shale samples with varying carbonate, clay and silica contents. An increase in the amorphous content, from 37% to 41.3%, of silica-rich and carbonate/clay lean shale is noted due to reactions with an acidic solution which is attributed to the dissolution of Si-bearing phases such as clays, accompanied by SiO 2 precipitation. In shales bearing high content of clays and carbonates, significant increase in the pore volumes and surface areas are noted. Non-monotonic changes in the micron-scale porosity of silica rich–carbonate/clay lean (e.g., Mowry shale) are noted using in-situ X-ray microtomography experiments. Due to the initial mobilization of silica and dissolution of carbonate/clay phases, the total porosity slightly increases from 6.7% to 10.7% followed by a decrease to similar to 4% caused by SiO 2 reprecipitation. In conclusion, these findings suggest that even though silica is less reactive in acidic environments, the changes in the amorphous and crystalline content due to dissolution and reprecipitation alter the porosity and fluid flow paths.

04 OIL SHALES AND TAR SANDS↗

Distribution of Mn Oxidation States in Grassland Soils and Their Relationships with Soil Pores

Manganese (Mn) is known to be an active contributor to processing and cycling of soil organic carbon (C), yet the exact mechanisms behind its interactions with C are poorly understood. Plant diversity in terrestrial ecosystems drives feedback links between plant C inputs and soil pores, where the latter, in turn, impact the redox environment and Mn. This study examined associations between soil pores (>36 μm Ø) and Mn within intact soils from two grassland ecosystems, after their >6-year implementation in a replicated field experiment. In this work, we used μ-XRF imaging and XANES spectroscopy to explore spatial distribution patterns of Mn oxidation states, combined with X-ray computed microtomography and 2D zymography. A high plant diversity system (restored prairie) increased soil C and modified spatial distribution patterns of soil pores as compared to a single species system (monoculture switchgrass). In switchgrass, the abundance of oxidized and reduced Mn oxidation states varied with distance from pores consistently with anticipated O 2 diffusion, while in the soil from restored prairie, the spatial patterns suggested that biological activity played a greater role in influencing Mn distributions. Based on the findings, we propose a hypothesis that Mn transformations promote C gains in soils of high plant diversity grasslands.

54 ENVIRONMENTAL SCIENCES↗