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All sourcesNASA NTRSDOE OSTI
NASA NTRS2009

Multiplexed Colorimetric Solid-Phase Extraction

Multiplexed colorimetric solid-phase extraction (MC-SPE) is an extension of colorimetric solid-phase extraction (C-SPE) an analytical platform that combines colorimetric reagents, solid phase extraction, and diffuse reflectance spectroscopy to quantify trace analytes in water. In CSPE, analytes are extracted and complexed on the surface of an extraction membrane impregnated with a colorimetric reagent. The analytes are then quantified directly on the membrane surface using a handheld diffuse reflectance spectrophotometer. Importantly, the use of solid-phase extraction membranes as the matrix for impregnation of the colorimetric reagents creates a concentration factor that enables the detection of low concentrations of analytes in small sample volumes. In extending C-SPE to a multiplexed format, a filter holder that incorporates discrete analysis channels and a jig that facilitates the concurrent operation of multiple sample syringes have been designed, enabling the simultaneous determination of multiple analytes. Separate, single analyte membranes, placed in a readout cartridge create unique, analyte-specific addresses at the exit of each channel. Following sample exposure, the diffuse reflectance spectrum of each address is collected serially and the Kubelka-Munk function is used to quantify each water quality parameter via calibration curves. In a demonstration, MC-SPE was used to measure the pH of a sample and quantitate Ag(I) and Ni(II).

Gazda, Daniel B.↗
NASA NTRS2012

The Search for Life on Mars - Current Knowledge, Earth Analogues, and Principal Issues

For centuries, the planet Mars has been imagined as a possible abode for life. Serious searches for life's signatures began in the 19th century via ground-based visual astronomy that stimulated a vibrant fantasy literature but little lasting scientific knowledge. Modern scientific inquiry has emphasized the search for chemical signatures of life in the soil and rocks at the planet's surface, and via biomarker gases in the atmosphere. Today, investigations are based on high-resolution spectroscopy at Earth's largest telescopes along with planet orbiting and landed space missions. Methane has assumed central importance in these searches. Living systems produce more than 900/0 of Earth's atmospheric methane; the balance is of geochemical origin. Abundant methane is not expected in an oxidizing atmosphere such as Mars', and its presence would imply recent release - whether biological or geochemical. F or that reason, the quest for methane on Mars has been a continuing thread in the fabric of searches conducted since 1969. I will review aspects of the discovery and distribution of methane on Mars, and will mention ongoing extended searches for clues to its origin and destruction. On Earth, hydrogen (generated via serpentinization or radiolysis of water) provides an important 'fuel' for carbonate-reducing and sulphate-reducing biota (CH4 and H2S producers, respectively). Several such communities are known to reside at depth in continental domains (e.g., Lidy Hot Springs, Idaho; Witwatersrand Basin, S. Africa). If similar conditions exist in favourable locations on Mars, organisms similar to these could likely prosper there. Geologic (abiotic) production will also be mentioned, especially abiotic methane production associated with low-temperature serpentinization (e.g., terrestrial ophiolites). It is vitally important to pursue evidence for geochemical and biological production with equal vigour and intellectual weight lest unwanted and unintended bias contaminate the results. Finally, I will touch upon unresolved questions and issues posed by the methane detections.

Mumma, Michael J.↗
NASA NTRS2019

Surface Biology & Geology Pathfinder Data Analysis Pipeline

NASA's future global orbital mission, currently in development as the Surface Biology and Geology (SBG) Designated Observable study, will acquire relatively high resolution solar-reflected spectroscopy and thermal infrared observations. Innovative processes must be utilized for handling the high volume of data anticipated to be collected, which is anticipated to exceed 100 terabytes/day, greater than NASA's total extant airborne hyperspectral data collection. Collecting, processing/re-processing, disseminating, and exploiting this volume of data presents new challenges. To begin addressing them, NASA is drawing upon the expertise developed from its astrophysics programs to address Earth science and applications. Specifically, NASA is adapting the science processing operations technology developed for the Kepler and TESS planet-hunting missions for imaging spectroscopy data processing. This technology development has been the foundation for the remarkable scientific successes of Kepler and TESS. The Kepler/TESS data processing technology provides a scalable architecture for robust, repeatable, and replicable science and application products while enabling the Earth science community to develop, test, and implement new algorithms. Our effort to leverage this existing capability has begun by ingesting data and applying workflows from the EO-1/Hyperion 17-year mission archive that provides globally sampled visible through shortwave infrared spectra that are representative of SBG data types and volumes. This pathfinding data processing system will help define the solutions to processing SBG data volumes and will enable the scientific community to interact with the data and processing pipeline to create new science products.

Jenkins, Jon↗
NASA NTRS2020

Using Simulated Micrometeoroid Impacts to Understand the Progressive Space Weathering of the Surface of Mercury

The surfaces of airless bodies such as Mercury are continually modified by space weathering, which is driven by micrometeoroid impacts and solar wind irradiation. Space weathering alters the chemical composition, microstructure, and spectral properties of surface regolith. In lunar and ordinarychondritic style space weathering, these processes affect the reflectance properties by darkening (lowering of reflectance), reddening (increasing reflectance with increasing wavelength), and attenuation of characteristic absorption features. These optical changes are driven by the production of nanophase Febearing particles (npFe). While our understanding of these alteration processes has largely been based on data from the Moon and near-Earth S-type asteroids, the space weathering environment at Mercury is much more extreme. The surface of Mercury experiences a more intense solar wind flux and higher velocity micrometeoroid impacts than its planetary counterparts at 1 AU. Additionally, the composition of Mercury’s surface varies significantly from that of the Moon. Most notably, a very low albedo unit has been identified on Mercury’s surface, known as the low reflectance material (LRM). This unit is enriched with up to 4 wt.% carbon, likely in the form of graphite, over the local mean. In addition, the surface concentration of Fe across Mercury’s surface is low (<2 wt.%) compared to the Moon. Our understanding of how these low-Fe and carbon phases are altered as a result of space weathering processes is limited. Since Fe plays a critical role in the development of space weathering features on other airless surfaces (e.g., npFe), its limited availability on Mercury may strongly affect the space weathering features in surface materials. In order to understand how space weathering affects the chemical, microstructural, and optical properties of the surface of Mercury, we can simulate these processes in the laboratory [7]. Here we used pulsed laser irradiation to simulate the short duration, high temperature events associated with micrometeoroid impacts. We used forsteritic olivine, likely present on the Mercurian surface, with varying FeO contents, each mixed with graphite, in our experiments. We then performed reflectance spectroscopy and electron microscopy to investigate the spectral, chemical, and microstructural changes in these samples.

Thompson, Michelle S.↗
NASA NTRS2023

The Earth in Living Color - NASA’s Surface Biology and Geology Designated Observable

The Surface Biology and Geology (SBG) Designated Observable will transform our understanding of the global land surface, inland and coastal aquatic ecosystems through visible-to-shortwave infra-red imaging (VSWIR) spectroscopy and thermal infra-red (TIR) imaging. SBG is one of four high-priority observables recommended in the 2017 NASA Earth Science Decadal Survey t o address science questions on vegetation and aquatic ecosystem health, snow-cover dynamics, volcanic activity, and minerology. With a planned launch readiness date of 2028, SBG is currently in Pre-Phase A, with Level 1 requirements being developed for a two-spacecraft architecture, including an additional constellation pathfinder. The recommended architecture emerged from an extensive study (2018-2021) that engaged the research and applications community to consider the science questions and measurement objectives of the Decadal Survey. A Science and Applications Traceability Matrix was used as a basis for scoring candidate architectures, with inputs from four working groups that covered algorithms, applications, calibration and validation, and modeling. Two pathfinder studies, Modeling End-to-End Traceability in support of SBG (MEET-SBG) and Space-based Imaging Spectroscopy and Thermal pathfindER (SISTER) are providing pre-launch modeling tools and data for algorithm development to support science value trades. The architecture consists of one spacecraft hosting a wide-swath VSWIR imaging spectrometer providing 30-m ground-sample distance (GSD), a spectral range of 380-2500 nm (at 10 nm resolution), 16-day revisit with 400 signal-to-noise for VNIR and 250 for SWIR (at 25% reflectance). A separate spacecraft will host a wide swath thermal imager, with five to seven bands placed between 4-12 μm), with 60-m (GSD), 3- day revisit, and 0.2K noise-equivalent differential temperature (NeDT). A VNIR compact camera will be hosted on the TIR spacecraft to enable coincident TIR and VNIR observations. A constellation pathfinder will evaluate options for enabling VSWIR mission continuity using Small Sats or data buys. Partnerships with international space agencies contribute technology as well as improvements to temporal revisit. SBG, when launched, will be the first dedicated mission collecting the full spectra of the Earth’s ‘living color’ and will play a critical role in NASA’s Earth System Observatory.

David S Schimel↗
NASA NTRS1979

Effect of nitrogen-containing plasma on adherence, friction, and wear of radiofrequency-sputtered titanium carbide coatings

Friction and wear experiments on 440C steel surfaces that were rf sputtered with titanium carbide when a small percentage of nitrogen was added to the plasma were conducted. Both X-ray photoelectron spectroscopy and X-ray diffraction were used to analyze the resultant coatings. Results indicate that the small partial pressure of nitrogen (approximately 0.5 percent) markedly improves the adherence, friction, and wear properties when compared with coatings applied to sputter-etched surfaces, oxidized surfaces, or in the presence of a small oxygen partial pressure. The improvements are related to the formation of an interface containing a mixture of the nitrides of titanium and iron, which are harder than their corresponding oxides.

Brainard, W. A.↗
NASA NTRS1979

Proportional counter for X-ray analysis of lunar and planetary surfaces

A position sensitive proportional scintillation detector was developed and evaluated for use in applications involving X-ray imaging as well as spectroscopy. Topics covered include limitations of the proportional scintillation counter for use in space; purification of the xenon gas in the detector, and the operation of the detector system. Results show that the light signal in a proportional scintillation detector remains well localized. With modest electric fields in xenon, the primary electrons from a photoelectric absorption of an X-ray can be brought a distance of a few millimeters to a higher field region without spreading more than a millimeter or so. Therefore, it is possible to make a proportional scintillation detector with good position sensitivity that could be used to calibrate out the difference in light collection over its sensitive volume.

Source record↗
NASA NTRS1990

Quantitative analysis of ice films by near-infrared spectroscopy

One of the outstanding problems in the Space Transportation System is the possibility of the ice buildup on the external fuel tank surface while it is mounted on the launch pad. During the T-2 hours (and holding) period, the frost/ice thickness on the external tank is monitored/measured. However, after the resumption of the countdown time, the tank surface can only be monitored remotely. Currently, remote sensing is done with a TV camera coupled to a thermal imaging device. This device is capable of identifying the presence of ice, especially if it is covered with a layer of frost. However, it has difficulty identifying transparent ice, and, it is not capable of determining the thickness of ice in any case. Thus, there is a need for developing a technique for measuring the thickness of frost/ice on the tank surface during this two hour period before launch. The external tank surface is flooded with sunlight (natural or simulated) before launch. It may be possible, therefore, to analyze the diffuse reflection of sunlight from the external tank to determine the presence and thickness of ice. The purpose was to investigate the feasibility of this approach. A near-infrared spectrophotometer was used to record spectra of ice. It was determined that the optimum frequencies for monitoring the ice films were 1.03 and 1.255 microns.

Keiser, Joseph T.↗
NASA NTRS1982

Surface analysis in composite bonding

The role of the interfacial region in determining the bond strength and durability of composite bonds is discussed. The characterization of a variety of carbon fibers including Celion 6000 using both scanning electron microscopy and X-ray photoelectron spectroscopy is discussed. The emphasis is on composite bonding, that is, the adhesive bonding between composites in contrast to fiber-matrix interaction. The primary objective of the research is the characterization of composite surfaces before adhesive bonding and after fracture of bonded specimens. Work done on the analysis of composite samples pretreated in a number of ways prior to bonding is detailed.

Messick, D. L.↗
NASA NTRSDate not supplied

Spectroscopy of Mount Etna Lava Flows as A Proxy for Age: A Potential Analogue to Recent Volcanism on Venus

There is growing evidence of geologically recent volcanism at Venus [1–3], a question that may be resolved by forthcoming missions to our sister planet that will make spectroscopic measurements of the surface. The thick, relatively opaque atmosphere of Venus makes observation difficult, but a few key atmospheric windows in the near-infrared (NIR) around 1 μm make emission from the surface detectable [4]. At these wavelengths, the spectroscopic signature of rocks are due to its primary mineralogy and chemistry, as well as the presence of secondary weathering minerals [2, 5, 6]. If the degree of alteration can be tied to the spectroscopy of Venus analogue materials, then spectroscopy of venusian lava flows can potentially reveal their degree of weathering and thus their age, which in turn gives an estimate of the extent of recent volcanism [2, 7]. A potential Earth analogue to volcanoes on Venus is Mount Etna in Sicily, Italy [8]. This composite volcano is among the most active in the world and features mafic lava flows with definitive ages that exhibit varying degrees of alteration [9]. While Mount Etna is not a perfect analogue due to its different weathering environment, the natural age progression of altered basaltic rock can be a useful comparison. Here, we will investigate how weathering at Mount Etna affects spectroscopic measurements and if this can be used as a proxy for Venus. While planned missions to Venus such as DAVINCI, VERITAS, and EnVision will measure NIR emissivity from the surface, Kirchhoff’s Law states that e = 1 − r, where e is emissivity and r is reflectance, meaning that NIR emissivity can be estimated from reflectance measurements [10]. Given its relative ease, laboratory reflectance spectroscopy is a useful tool to efficiently test potential Venus analogue materials.

Gabriel L Eggers↗
NASA NTRS1981

Chemical composition of the SiO2/InSb interface as determined by X-ray photoelectron spectroscopy

In connection with the relatively poor insulating characteristics of the native oxides of most III-V compound semiconductors, there has been interest in the development of deposited dielectric layers for surface passivation and MOS device fabrication on III-V compound semiconductor substrates. The chemical system of SiO2 deposited on single-crystal InSb substrates has been proposed for the fabrication of IR CCD. The considered investigation is concerned with a detailed examination of the chemical nature of the interactions between deposited and native oxides using X-ray photoelectron spectroscopy (XPS) in conjunction with a chemical-etching technique for depth profiling. The compositional structure of the interfaces obtained in the SiO2/native oxide/InSb system is derived on the basis of an intensity analysis of XPS spectra. Thermal oxidation of the InSb substrate is found to result in an In-rich native oxide and excess elemental Sb at the native oxide/substrate interface.

Vasquez, R. P.↗
NASA NTRSDate not supplied

Revisiting the Origin of Macromolecular Carbon (MMC) in Lunar Basalts 15556 & 10044

Volatile elements influence the geo-chemical evolution of planetary bodies and they are in magmas at every stage, from melting within planetary interiors to eruption at the surface. Analyses of lunar mare basalts supported the hypothesis that lunar mag-mas were depleted in volatiles (H-C-F-Cl-S), relative to their terrestrial analogs [1]. Nevertheless, several early studies of samples returned during the Apollo program proposed that the mare basalt eruptions, including the “fire fountain” eruptions, were propelled by the oxidation of magmatic graphite to CO (and/or CO2) gas [2, 3]. Seminal studies during the 1970’s measured the bulk concentration and isotopic compositions of C from Apollo 11 samples, and identified several carbonaceous compounds, including: (a) gaseous (CO, CO2, and traces of CH4), (b) metallic carbide, and (c) potentially elemental carbon [4-6]. These studies reported a relatively broad range of C contents (~100-400 μg/g) and isotopic values (δC13 = -30 to +20), and suggested that these heterogeneities can be explained by contribution from multiple factors, including: (a) indigenous carbon, (b) solar wind implantation, (c) bombardment and/or meteorite impact, and (d) terrestrial contamination [5,6]. However, unequivocal observations of magmatic graphite in lunar basalts have never been made. Macromolecular carbon (MMC)—graphitic carbon varying from nearly amorphous to highly crystalline varieties—was identified as inclusions hosted by igneous pyroxenes from Martian meteorites and were attributed to being indigenous to Mars [8]. The authors carefully considered the textural and mineralogical relationship of the MMC phases, and concluded that the subset of MMC located within and/or adjacent to cracks, or at a disrupted surface (e.g., cut) were most consistent with terrestrial contamination. The near absence of con-firmed instances of lunar magmatic MMC within the literature [9], combined with the wide range of isotopic values and bulk carbon contents measured in lunar bas-alts begs the question as to whether previously measured carbon is of an indigenous origin, or the result of terrestrial contamination. Using Raman spectroscopy, we have observed MMC in lunar basalts subjected to different forms of anthropogenic modification related to sample preparation including polished sections, sawn surfaces, and fractured surfaces adjacent to sawn sur-faces. We have observed MMC of unknown origin in all of these settings. Here we report the preliminary textural and spectroscopic characteristics of MMC hosted within the groundmass of Apollo 15 (15556) and Apollo 11 basalts (10044) as part of our ongoing investigation of the origin of these carbonaceous materials.

lunar↗
NASA NTRS1979

Use of a nitrogen-argon plasma to improve adherence of sputtered titanium carbide coatings on steel

Friction and wear experiments on 440-C steel surfaces that had been RF-sputtered with titanium carbide when a small percentage of nitrogen was added to the plasma were conducted. X-ray photoelectron spectroscopy and X-ray diffraction were used to analyze the resultant coatings. Results indicate that a small partial pressure of nitrogen (about 0.5%) markedly improves the adherence, friction, and wear properties when compared with coatings applied on sputter-etched oxidized surfaces or in the presence of a small oxygen partial pressure. The improvements are related to the formation of an interface containing a mixture of the nitrides of titanium and iron, which are harder than their corresponding oxides.

Brainard, W. A.↗
NASA NTRS1992

Effects of the low Earth orbit space environment on the surface chemistry of Kapton polyimide film: An XPS study

Kapton H (DuPont Trademark) polyimide specimens exposed to the low earth (LEO) space environment suffered significant weathering with surface erosions of approximately 8.0 microns. Despite these effects, no significant changes in bulk chemistry were observed. X-ray photoelectron spectroscopy (XPS) was used to determine local changes induced from approximately 25 percent in 1980 vintage ground control specimens to nearly 53 percent in space exposed specimens. The greatest increase was observed for the divalent oxygen moieties, although a slight increase in carbonyl oxygen was also measured. Furthermore, the chemical shifts of all XPS peaks of space-exposed Kapton are shifted to higher energy. This is consistent with a higher oxidation state of the space exposed surface. Finally, space exposed specimens had distinct silicon peaks (2p 100 eV and 2s 149 eV) in their XPS spectra in agreement with widespread reports of silicon contamination throughout the LDEF satellite. These results are discussed in terms of surface reactivity of the polyimide exposed to the LEO environment and the chemical nature of contaminants deposited on flight surfaces due to satellite outgassing.

Lee, Myung↗
NASA NTRS1985

SEM/XPS analysis of fractured adhesively bonded graphite fibre-reinforced polyimide composites

The surfaces of the graphite fiber-reinforced polyimide composites presently pretreated prior to bonding with polyimide adhesive contained variable amounts of a fluoropolymer, as determined by X-ray photoelectron spectroscopy. Lap shear strengths were determined for unaged samples and for those aged over 500- and 1000-hour periods at 177 and 232 C. Unaged sample lap strengths, which were the highest obtained, exhibited no variation with surface pretreatment, but a significant decrease is noted with increasing aging temperature. These thermally aged samples, however, had increased surface fluorine concentration, while a minimal concentration was found in unaged samples. SEM demonstrated a progressive shift from cohesive to adhesive failure for elevated temperature-aged composites.

Devilbiss, T. A.↗
NASA NTRS1993

The dregs of crystallization in Zagami

The Zagami shergottite is a basaltic meteorite which formed when a phenocryst-bearing lava flow was emplaced at or near the surface of Mars. Recently, a cm-sized olivine-rich lithology has been identified in Zagami by Mossbauer spectroscopy. Olivine is extremely rare in shergottites, particularly in Zagami and Shergotty, where it occurs only as minute grains. We report petrologic and microprobe studies of this olivine-rich lithology. This material represents the last few percent of melt and is highly enriched in phosphates, opaques and mesostases, all of which are late-stage crystallization products. Phosphates replaced augite as a phenocryst phase when the magma became saturated in P. This late stage melt also includes a fayalite-bearing, multi-phase intergrowth which crystallized after the melt became too rich in iron to crystallize pigeonite. We can now reconstruct the entire crystallization history of the Zagami shergottite from a deep-seated magma chamber to crystallization of the final few percent of melt in a near-surface dike or thick flow. Small pockets (tens of microns) of late-stage melt pockets are ubiquitous but volumetrically minor in Zagami. We do not know the physical relationship between these areas and the cm-sized olivine-rich material described here. It is possible that these small pockets were mobile, forming larger areas. Perhaps inspection of the entire hand specimen of Zagami would clarify this relationship.

Mccoy, T. J.↗
NASA NTRS2002

Micro-Cracking Detection in Laminated Composites

Porosity and fatigue cracking are two critical factors that affect the performance and safety of cryogenic fuel tanks and feedlines made from unlined laminated or weaved carbon/epoxy materials. This paper presents the experiments to induce fatigue cracking of laminated composites through thermal cycling as well as the feasibility of using Thermography and Ultrasound Spectroscopy technology (UT) to detect and measure such micro-cracking. Carbon/epoxy laminated composite panels were built and cut into strips. These specimens were partially submerged in liquid nitrogen while subjected to various loads on a test machine. Edges of some specimens were polished and etched to determine the degree of micro-cracking. The rest of specimens were then examined with Thermography and Ultrasound Spectroscopy NDE systems to investigate the feasibility of finding such micro-cracking in the laminated composites. Thermography is utilized to determine changes in thermal diffusivity. The degree of cracking may reduce the apparent thermal diffusivity and therefore change the thermal response on the surface. Thermography testing was conducted on a group of specimens where it is desired to have some correlation between the predetermined stress and the thermography data. Ultrasound Spectroscopy was used to determine peak changes between the pre-stressed and stressed samples. Data from the inspections were analyzed and the results are presented in this paper.

Chu, Tsuchin↗
NASA NTRS2004

Moessbauer Spectroscopy of Soils and Rocks at Gusev Crater and Meridiani Planum

For the first time in history a Moessbauer spectrometer was placed on the surface of another planet. The miniaturized Moessbauer spectrometer MIMOS II is part of the Athena payload of NASA's twin Mars Exploration Rovers (MER) Spirit,and Opportunity. It determines the Fe-bearing mineralogy of Martian soils and rocks at the Rovers respective landing sites, Gusev crater and Meridiani Planum. First results of soil and rock measurements at both landing sites confirm a generally basaltic composition of Martian surface materials.

Klingelhoefer, G.↗