Fluorescent Probe of Aminopolymer Mobility in Bulk and in Nanoconfined Direct Air CO 2 Capture Supports
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36 MATERIALS SCIENCE↗
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In-Situ XRD/XRF to Support Life Detection on Mars
X-ray diffraction / X-ray fluorescence (XRD/XRF) analysis provides the most comprehensive mineralogical / compositional characterization of rocks and soils of any flight-capable technique. XRD data provide quantitative mineralogy (including abundance of X-ray amorphous materials) and crystal chemistry (structure, elemental composition and valence state), and XRF data provide complimentary major, minor, and some trace element abundances. Both types of data are important in evaluating habitability (environment of formation) and biosignature preservation/degradation (post-depositional diagenetic change). Whether or not a relict biosignature is detected, the mineral assemblage and its geochemistry can be used to determine the habitability of an ancient environment (e.g., salinity, pH, temperature), and to identify potential sources of energy for life (e.g., elements in different redox states). In this respect, a null result (a habitable environment lacking evidence of life) can play an important role in constraining the parameters of the search. Conversely, diagenetic alteration (taphonomic change) resulting from post-depositional variations in temperature, pressure or fluid chemistry can preserve evidence of biogenicity, erase such evidence completely or indeed can provide for post-depositional habitable conditions in the subsurface. XRD / XRF data are critical to these determinations. The CheMin instrument on the Mars Science Laboratory (MSL) Curiosity rover is the first XRD instrument flown in space. CheMin operates in transmission geometry with a Co X-ray source to minimize fluorescence from iron. Diffracted photons are collected with an energy-sensitive charge-coupled device (CCD). The position of the diffracted photons provides structural information for minerals, whereas the energy of sample-generated X-ray fluorescence photons provides elemental information, though these XRF data are qualitative. Mineralogical data from the CheMin XRD identified the three circumstances above: habitable depositional environments (e.g., Yellowknife Bay), habitable subsurface/diagenetic environments (e.g., throughout the Murray formation), and diagenetic conditions that may destroy evidence of habitability (e.g., oxidative and acidic environments at Vera Rubin ridge). Technological advances in X-ray technology and lessons learned from the operation of CheMin on Mars have resulted in a next-generation XRD/XRF, called CheMinX. Replacement of CheMin’s CCD with an array of hybrid pixel detectors and improvements in focusing optics dramatically decrease analysis time (15 minutes vs. 22 hours for MSL-CheMin) and result in a better angular resolution (0.18 vs. 0.30 °2θ for MSL-CheMin). This increased resolution improves mineral detection, including discrimination between types of pyroxenes, which is not possible with MSL-CheMin data. The hybrid pixel detectors do not require cooling like the MSL-CheMin CCD, therefore reducing the power needed to operate CheMinX. CheMinX has a silicon-drift detector (SDD) to measure fluoresced photons, enabling the quantification of major, minor, and some trace elements via XRF. XRD/XRF data are collected simultaneously in CheMinX, obviating the need for multiple compositional instruments. The CheMinX design also improves upon MSL-CheMin’s sample handling. Instead of sample cells on wheel, which are often not reusable and add complexity in commanding the instrument, CheMinX has single-use cells in a cartridge/dispenser configuration. Because of these improvements, CheMinX is an ideal instrument for Discovery-class life-detection missions, including Mars Life Explorer that was recommended for development in the Planetary Science and Astrobiology Decadal Survey 2023-2032.
E B Rampe↗
Development of an X-ray surface analyzer for planetary exploration
An ultraminiature X-ray fluorescence spectrometer was developed which can obtain data on element composition not provided by present spacecraft instrumentation. The apparatus employs two radioisotope sources (Fe-55 and Cd-109) which irradiate adjacent areas on a soil sample. Fluorescent X-rays emitted by the sample are detected by four thin-window proportional counters. Using pulse-height discrimination, the energy spectra are determined. Virtually all elements above sodium in the periodic table are detected if present at sufficient levels. Minimum detection limits range from 30 ppm to several percent, depending upon the element and the matrix. For most elements, they are below 0.5 percent. Accuracies likewise depend upon the matrix, but are generally better than plus or minus 0.5 percent for all elements of atomic number greater than 14. Elements below sodium are also detected, but as a single group.
Clark, B. C.↗
Measurements of aerosol microphysical and chemical properties in the central Arctic atmosphere during MOSAiC
The Arctic environment is transforming rapidly due to climate change. Aerosols’ abundance and physicochemical characteristics play a crucial, yet uncertain, role in these changes due to their influence on the surface energy budget through direct interaction with solar radiation and indirectly via cloud formation. Importantly, Arctic aerosol properties are also changing in response to climate change. Despite their importance, year-round measurements of their characteristics are sparse in the Arctic and often confined to lower latitudes at Arctic land-based stations and/or short high-latitude summertime campaigns. Here, we present unique aerosol microphysics and chemical composition datasets collected during the year-long Multidisciplinary drifting Observatory for the Study of Arctic Climate (MOSAiC) expedition, in the central Arctic. These datasets, which include aerosol particle number concentrations, size distributions, cloud condensation nuclei concentrations, fluorescent aerosol concentrations and properties, and aerosol bulk chemical composition (black carbon, sulfate, nitrate, ammonium, chloride, and organics) will serve to improve our understanding of high-Arctic aerosol processes, with relevance towards improved modelling of the future Arctic (and global) climate.
54 ENVIRONMENTAL SCIENCES↗
NASAs Evolvable Mars Campaign: Mars Moons Robotic Precursor
Human exploration missions to the moons of Mars are being considered within NASA's Evolvable Mars Campaign (EMC) as an intermediate step for eventual human exploration and pioneering of the surface of Mars. A range of mission architectures is being evaluated in which human crews would explore one or both moons for as little as 14 days or for as long as 500 days with a variety of orbital and surface habitation and mobility options being considered. Relatively little is known about the orbital, surface, or subsurface characteristics of either moon. This makes them interesting but challenging destinations for human exploration missions during which crewmembers must be able to effectively conduct scientific exploration without being exposed to undue risks due to radiation, dust, micrometeoroids, or other hazards. A robotic precursor mission to one or both moons will be required to provide data necessary for the design and operation of subsequent human systems and for the identification and prioritization of scientific exploration objectives. This paper identifies and discusses considerations for the design of such a precursor mission based on current human mission architectures. Objectives of a Mars' moon precursor in support of human missions are expected to include: 1) identifying hazards on the surface and the orbital environment at up to 50-km distant retrograde orbits; 2) collecting data on physical characteristics for planning of detailed human proximity and surface operations; 3) performing remote sensing and in situ science investigations to refine and focus future human scientific activities; and 4) prospecting for in situ resource utilization. These precursor objectives can be met through a combination or remote sensing (orbital) and in-situ (surface) measurements. Analysis of spacecraft downlink signals using radio science techniques would measure the moon's mass, mass distribution, and gravity field, which will be necessary to enable trajectory planning. Laser altimetry would precisely measure the moon's shape and improve the accuracy of radio science measurements. A telescopic imaging camera would map the moon at submeter resolution and photograph selected areas of interest at subcentimeter resolution and a visible and near-infrared (0.4-3.0 mm) imaging spectrograph would produce a global map of mineral composition variations at a resolution of tens of meters and maps of selected areas of interest at meter resolution. Additional remote sensing capabilities could include a thermal infrared imager (heat flow, thermal inertia, and grain size distributions), a gamma-ray and neutron detector (atomic composition), a ground-penetrating radar (internal structure), and a magnetometer and Langmuir probe (magnetic properties and plasma field). Once on the surface of Phobos or Deimos, necessary instrumentation would include a penetrometer (regolith compressive strength), a motion-imagery camera (to observe the penetrometer tests before, during, and after contact), a dust-adhesion witness plate and camera (dust levitation), a microimager (dust particle sizes and shapes), and an alpha-proton-X-ray, X-ray fluorescence, Mossbauer, or Raman spectrometer (atomic and mineral composition of surface materials) and an optional temperature probe (regolith thermal properties). A variety of robotic mission design options to enable both orbital and surface measurements are being considered that include fully integrated and modular approaches. In-situ measurements from at least one surface location would be required, with additional measurement locations possible through use of multiple landers, through propulsive relocation of a single lander, or through electromechanical surface translation by a walking or hopping lander vehicle, which could also serve to evaluate such mobility capabilities for subsequent human missions. Preliminary orbital analysis suggests that remote sensing would likely be performed while in a distant retrograde orbit around the target moon. Mission design options to enable characterization of both Mars’ moons in a single mission are also being studied.
Gernhardt, Michael L.↗
Multimodal Imaging of Autofluorescent Sites Reveals Varied Chemical Speciation in SSZ-13 Crystals
In this report a multimodal imaging study of chabazite is used to analyse emissive deposits. A notable difference is seen in the morphology of agglomerated surface deposits and larger subsurface deposits. Comparison of the distribution of organic residue throughout the crystal volume and XRF mapping is demonstrating that a fluorescence-based technique can also be used to indirectly comment on the compositional chemistry of the inorganic framework. A multimodal imaging study of chabazite is used to show the distribution of and discriminate between different emissive deposits arising as a result of the detemplation process. Confocal imaging, 3D fluorescence lifetime imaging, 3D multispectral fluorescence imaging, and Raman mapping are used to show three different types of emissive behaviours each characterised by different spatial distributions, trends in lifetime, spectral signals, and Raman signatures. A notable difference is seen in the morphology of agglomerated surface deposits and larger subsurface deposits, which experience lifetime augmentation due to spatial confinement. The distribution of organic residue throughout the crystal volume is comparable to XRF mapping that shows Si enrichment on the outer edges and higher Al content through the centre, demonstrating that a fluorescence-based technique can also be used to indirectly comment on the compositional chemistry of the inorganic framework.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Estimation of Supraglacial Dust and Debris Geochemical Composition via Satellite Reflectance and Emissivity
We demonstrate spectral estimation of supraglacial dust, debris, ash and tephra geochemical composition from glaciers and ice fields in Iceland, Nepal, New Zealand and Switzerland. Surface glacier material was collected and analyzed via X-ray fluorescence spectroscopy (XRF) and X-ray diffraction (XRD) for geochemical composition and mineralogy. In situ data was used as ground truth for comparison with satellite derived geochemical results. Supraglacial debris spectral response patterns and emissivity-derived silica weight percent are presented. Qualitative spectral response patterns agreed well with XRF elemental abundances. Quantitative emissivity estimates of supraglacial SiO2 in continental areas were 67% (Switzerland) and 68% (Nepal), while volcanic supraglacial SiO2 averages were 58% (Iceland) and 56% (New Zealand), yielding general agreement. Ablation season supraglacial temperature variation due to differing dust and debris type and coverage was also investigated, with surface debris temperatures ranging from 5.9 to 26.6 C in the study regions. Applications of the supraglacial geochemical reflective and emissive characterization methods include glacier areal extent mapping, debris source identification, glacier kinematics and glacier energy balance considerations.
Casey, Kimberly Ann↗
Biomimetic tissue phantoms for neurosurgical near-infrared fluorescence imaging
Neurosurgical fluorescence imaging is a well-established clinical approach with a growing range of indications for use. However, this technology lacks effective phantom-based tools for development, performance testing, and clinician training. Our primary aim was to develop and evaluate 3D-printed phantoms capable of optically and morphologically simulating neurovasculature under fluorescence angiography. Volumetric digital maps of the circle of Willis with basilar and posterior communicator artery aneurysms, along with surrounding cerebral tissue, were generated. Phantoms were fabricated with a stereolithography printer using custom photopolymer composites, then visualized under white light and near-infrared fluorescence imaging. Feature sizes of printed components were found to be within 13% of digital models. Phantoms exhibited realistic optical properties and convincingly recapitulated fluorescence angiography scenes. Methods identified in this study can facilitate the development of realistic phantoms as powerful new tools for fluorescence imaging.
3D modeling↗
Constraints on Martian Soil Composition as Inferred from Viking XRFS and Pathfinder APXS and IMP Data
With the successful operation of the Alpha Proton X-Ray Spectrometer (APXS) during 1997's Mars Pathfinder (MPF) mission, geochemistry data are now available from three sites on Mars. APXS raw spectra for six soils and five rocks have been converted to compositional abundances. The Viking Lander X-Ray Fluorescence Spectrometer (XRFS) successfully measured elemental abundances of nine soils at Viking 1 and eight soils at Viking 2. Although the three landing sites are located in different parts of Mars, the soils exhibit broad similarities, with an iron-rich chemistry similar to that of palagonite. However, the Pathfinder sods show some significant differences from Viking soils, notably an enrichment in silica and depletion in sulfur. The XRFS samples consisted of near-surface and deep (up to 22 cm) soils acquired by a collector head at the cod of a retractable boom. It was possible to collect and analyze pebbles as large a 2 cm, but only sod, some in the form of consolidated clods, was sampled. In contrast, the APXS measured materials in situ. This resulted in MPF "rock" analyses that probably had a significant dust component and, as explored here, "soil" analyses that may have contained a rocky component We examine several possibilities to explain these differences and other attributes of the APXS and XRFS data sets: 1) The APXS soil measurements actually sampled a mixture of Viking-like soil and small bits of high-silica, low-sulfur rock, 2) The soils were derived from high-silica rocks mixed with a minor component of globally-homogenized dust; these soils are chemically distinct and have a separate geologic history from the Viking soils. 3) The weathering environment was different at the Pathfinder landing site compared to the Viking sites, and 4) Uncertainties in the XRFS and APXS measurements result in reported elemental abundances different than those that are actually present We show that none of the possibilities can be discounted, but that an MPF soil distinct in composition from Viking sods is best supported by the available data.
Bridges, N. T.↗
The diversity of aluminum-based drinking water treatment residuals for use in environmental remediation
Drinking water treatment residuals (DWTRs) are complex mixtures of organic and inorganic phases generally disposed of as waste materials. However, their strong sorptive properties could be further exploited to immobilize contaminants. To characterize these materials, we applied a range of analytical techniques to a set of aluminum-based DWTRs. Here we determined surface areas, elemental compositions using CHNS analysis and X-ray fluorescence (XRF), performed thermogravimetric analyses paired with mass spectrometry (TGA-MS), and used synchrotron-based methods: X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS). Elemental analyses and specific surface area measurements – that vary between 7.23 ± 0.03 and 197.6 ± 0.9 m 2 g –1 – indicate that non-coagulant additives must play an important role in controlling sorption. High resolution powder XRD reveals the presence of only a few crystalline minerals mostly derived from source waters or additives. Fe was detected by XRF in all samples, whereas Mn was present in significant levels in samples with potassium permanganate as additive. The chemical speciation of these elements was characterized by performing spectral decompositions of XAS spectra. The spectral features of Fe are consistent with iron(III) oxides/hydroxides and structural iron in clays. On the other hand, Mn is predominantly present under its reduced form, Mn(II).
54 ENVIRONMENTAL SCIENCES↗
Physical and chemical properties of the Martian soil: Review of resources
The chemical and physical properties of Martian surface materials are reviewed from the perspective of using these resources to support human settlement. The resource potential of Martian sediments and soils can only be inferred from limited analyses performed by the Viking Landers (VL), from information derived from remote sensing, and from analysis of the SNC meteorites thought to be from Mars. Bulk elemental compositions by the VL inorganic chemical (x ray fluorescence) analysis experiments have been interpreted as evidence for clay minerals (possibly smectites) or mineraloids (palagonite) admixed with sulfate and chloride salts. The materials contained minerals bearing Fe, Ti, Al, Mg and Si. Martian surface materials may be used in many ways. Martian soil, with appropriate preconditioning, can probably be used as a plant growth medium, supplying mechanical support, nutrient elements, and water at optimal conditions to the plants. Loose Martian soils could be used to cover structures and provide radiation shielding for surface habitats. Martian soil could be wetted and formed into abode bricks used for construction. Duricrete bricks, with strength comparable to concrete, can probably be formed using compressed muds made from martian soil.
Stoker, C. R.↗
Chemical characterization of seven Large Area Collector particles by SXRF
Optical microscopy and synchrotron X-ray fluorescence (SXRF) are used to analyze the chemical composition of seven dark-appearing cosmic-dust particles obtained in the stratosphere during NASA Johnson Large Area Collector flights. The experimental setup and procedures are outlined, and the results are presented in extensive tables. Three of the particles had abundances similar to those of chondrites (except for low Ca values in one particle); two had a metallic appearance and spectra dominated by Fe and Zn; one contained Cu and Cr plus small amounts of Fe and Zn; and one had igneous-type abundances of minor and trace elements while containing all of the elements seen in chondritic particles, suggesting it may be of extraterrestrial origin.
Flynn, G. J.↗
Laboratory Astrophysics and Microanalysis with NTD-Germanium-Based X-Ray Microcalorimeter
With the ability to create cosmic plasma conditions in the laboratory it is possible to investigate the dependencies of key diagnostic X-ray lines on density, temperature, and excitation conditions that exist in astrophysical sources with X-ray optics and a high resolution x-ray microcalorimeter. The same instrumentation can be coupled to scanning electron microscopes or x-ray fluorescence probes to analyze the elemental and chemical composition of electronic, biological, geological and particulate materials. We describe how our microcalorimeter and x-ray optics provide significantly improved capabilities for laboratory astrophysics and microanalysis.
Silver, E.↗
The Apollo 15 X-ray fluorescence experiment
The CSM spectrometric data on the lunar surface with respect to its chemical composition are presented for Al, Mg, and Si as Al/Si and Mg/Si ratios for the various features overflow by the spacecraft. The lunar surface measurements involved observations of the intensity and characteristic energy distribution of the secondary or fluorescent X-rays produced by the interaction of solar X-rays with the lunar surface. The results showed that the highlands and maria are chemically different, with the highlands having considerably more Al and less Mg than the maria. The mare-highland contact is quite sharp and puts a limit on the amount of horizontal transport of material. The X-ray data suggest that the dominant rock type of the lunar highlands is a plagioclase-rich pyroxene bearing rock, probably anorthositic gabbro or feldspathic basalt. Thus the moon appears to have a widespread differentiated crust (the highlands) systematically richer in Al and lower in Mg than the maria. This crust is pre-mare and may represent the first major internal differentiation of the moon.
Adler, I.↗
Glycine betaine accumulation, ionic and water relations of red-beet at contrasting levels of sodium supply
Exposure of plants to sodium (Na) and salinity may increase glycine betaine accumulation in tissues. To study this, red-beet cvs. Scarlet Supreme and Ruby Queen, were grown for 42 days in a growth chamber using a re-circulating nutrient film technique with 0.25 mmol/L K and either 4.75 mmol/L (control) or 54.75 mmol/L (saline) Na (as NaCl). Plants were harvested at weekly intervals and measurements were taken on leaf water relations, leaf photosynthetic rates, chlorophyll fluorescence, chlorophyll levels, glycine betaine levels, and tissue elemental composition. Glycine betaine accumulation increased under salinity and this accumulation correlated with higher tissue levels of Na in both cultivars. Na accounted for 80 to 90% of the total cation uptake under the saline treatment. At final harvest (42 days), K concentrations in laminae ranged from approximately 65-95 micromoles g-1 dry matter (DM), whereas Na in shoot tissue ranged from approximately 3000-4000 micromoles g-1. Leaf sap osmotic potential at full turgor [psi(s100)] increased as lamina Na content increased. Glycine betaine levels of leaf laminae showed a linear relationship with leaf sap [psi(s100)]. Chlorophyll levels, leaf photosynthetic rates, and chlorophyll fluorescence were not affected by Na levels. These results suggest that the metabolic tolerance to high levels of tissue Na in red-beet could be due to its ability to synthesize and regulate glycine betaine production, and to control partitioning of Na and glycine betaine between the vacuole and the cytoplasm.
NASA Center KSC↗
Aqueous chemiluminescent systems
This invention relates to novel water-soluble esters of oxalic acid, and to compositions that are useful for generating chemiluminescent emission by reacting said esters of oxalic acid with hydrogen peroxide in the presence of water and a fluorescent compound, and to a process for generating chemiluminescent emission by using said compositions.
Mohan, Arthur Gaudens↗
X-ray fluorescence surface contaminant analyzer: A feasibility study
The bonding of liner material to the inner metal surfaces of solid rocket booster cases is adversely affected by minute amounts of impurities on the metal surface. Suitable non-destructive methods currently used for detecting these surface contaminants do not provide the means of identifying their elemental composition. The feasibility of using isotopic source excited energy dispersive X-ray fluorescence as a possible technique for elemental analysis of such contaminants is investigated. A survey is made of the elemental compositions of both D-6ac steel, a common construction material for the booster cases, and Conoco HD-2 grease, a common surface contamination. Source and detector choices that maximize signal to noise ratio in a Recessed Source Geometry are made. A Monte Carlo simulation is then made of the optimized device incorporating the latest available X-ray constants at the energy of the chosen source to determine the device's response to a D-6ac steel surface contained with Conoco HD-2 grease.
Eldridge, Hudson B.↗
Planetary exploration sensor systems
Most of the instruments that have been used in planetary exploration have been either spectrometers or imaging devices. Instruments of these types are being developed for the Galileo and VOIR (Venus Orbiting Imaging Radar) missions. Galileo will take advantage of new CCD (charge-coupled device) technology, and VOIR will use techniques of synthetic aperture radar developed for Seasat. For determining the macrostructure of mineral resources, the best approach is believed to involve acoustic imaging, essentially a seismic data processing technique. Determinations of microstructure would require a light microscope and an electron microscope. For determining the nature and form of volatiles, a differential scanning calorimeter could be used. To determine the mineral composition, an electron beam microprobe with X-ray fluorescence and spectroscopy would be used.
Saunders, R. S.↗