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NASA NTRS2024

Enantioselective Three-Dimensional High-Performance Liquid Chromatographic Determination of Amino Acids in the Hayabusa2 Returned Samples from the Asteroid Ryugu

The chirality of amino acids in extraterrestrial materials may provide an insight into the origin of the essential L-enantiopure amino acids in the terrestrial biosphere. In 2020, the Hayabusa2 mission succeeded in bringing back surface materials from the C-type asteroid (162173) Ryugu to the Earth. Amino acids were one of the targeted organic molecules to be studied in the Ryugu samples. To analyze the various structural isomers of amino acids, which were expected to be present, from the limited amount of the returned samples, the development of a highly-sensitive and selective analytical method was necessary. In the present study, a three-dimensional high-performance liquid chromatography (3D-HPLC) system has been developed for the enantioselective determination of five proteinogenic and three non-proteinogenic amino acids in the Ryugu samples, in which amino acids in the sample were separated by reversed-phase, anion-exchange and enantioselective columns after the fluorescence derivatization with 4-fluoro-7-nitro-2,1,3-benzoxadiozole. The applicability of the analytical system to the extraterrestrial samples was evaluated by analyzing several types of carbonaceous meteorites before applying the system to the Ryugu samples. In the analysis of the Ryugu samples, all of the target amino acids were successfully determined quantitatively. Non-proteinogenic amino acids including 2-amino-n-butyric acid, isovaline and norvaline, rarely present in the terrestrial environment, were found as almost racemic mixtures with 47.1 to 55.2%L.

Amino acids↗

NASA NTRS2003

Infrared Database for Process Support Materials

Process support materials' compatibility with cleaning processes is critical to ensure final hardware cleanliness and that performance requirements are met. Previous discovery of potential contaminants in process materials shows the need for incoming materials testing and establishment of a process materials database. The Contamination Control Team of the Materials, Processes, and Manufacturing (MP&M) Department at Marshall Space Flight Center (MSFC) has initiated the development of such an infrared (IR) database, called the MSFC Process Materials IR database, of the common process support materials used at MSFC. These process support materials include solvents, wiper cloths, gloves, bagging materials, etc. Testing includes evaluation of the potential of gloves, wiper cloths, and other items to transfer contamination to handled articles in the absence of solvent exposure, and the potential for solvent exposure to induce material degradation. This Technical Memorandum (TM) summarizes the initial testing completed through December 2002. It is anticipated that additional testing will be conducted with updates provided in future TMs.Materials were analyzed using two different IR techniques: (1) Dry transference and (2) liquid extraction testing. The first of these techniques utilized the Nicolet Magna 750 IR spectrometer outfitted with a horizontal attenuated total reflectance (HATR) crystal accessory. The region from 650 to 4,000 wave numbers was analyzed, and 50 scans were performed per IR spectrum. A dry transference test was conducted by applying each sample with hand pressure to the HATR crystal to first obtain a spectrum of the parent material. The material was then removed from the HATR crystal and analyzed to determine the presence of any residues. If volatile, liquid samples were examined both prior to and following evaporation.The second technique was to perform an extraction test with each sample in five different solvents.Once the scans were complete for both the dry transference and the extraction tests, the residue from each scan was interpreted.

Bennett, K. E.↗

NASA NTRS1986

Liquid crystals for high-altitude in-flight boundary layer flow visualization

A novel method for visualization of laminar to turbulent boundary layer transition in flight is presented, in which liquid crystal coatings are used to indicate the transition by a change of color (in response to the changes in the wall shear and the temperature). The liquid crystals applied to the wing surfaces were either cholesteric crystals formulated to be active between temperatures of 30 and 100 F or a sample of chiral nematic liquid crystals formulated to be active between -18 and -22 F. Liquid crystal coatings were shown to provide visualization data at flight altitudes and temperatures at which data could not be obtained previously. Flight evaluations were successfully conducted on a T-34C and a Learjet research aircraft at Mach numbers of up to 0.8 and altitudes of up to 50,000 ft. The time response during oscillating sideslip tests was very rapid. In wind tunnel tests, a hysteresislike behavior was observed in the liquid crystal coatings, possibly because of the lower dynamic pressures in wind tunnels as compared to flight.

Gall, P. D.↗

NASA NTRS1992

Supercooling effects in Cu-10 wt pct Co alloys solidified at different cooling rates

Electromagnetic levitation and electron beam surface melting were employed to study the effects of supercooling and cooling rate on the solidification of Cu-10 wt pct Co alloys. Two major effects were observed in the supercooled alloys: the nucleation of a metastable copper-rich phase which contains 13 wt pct to 20 wt pct Co in samples supercooled between 105 and 150 K and liquid phase separation which occurs in samples supercooled 150 K or more. The microstructure of the electron beam melted surfaces consisted of very fine spheres which were similar to those of the sample supercooled more than 150 K but with a refined microstructure. The results indicate that a dynamic bulk supercooling of 150 K may exist in the molten pool during the solidification of electron beam melted surfaces.

Munitz, A.↗

NASA NTRS1998

Void Management in MEPHISTO and Other Space Experiments

The second flight of NASA's Shuttle Flight experiment program known as MEPHISTO suffered from a void in the liquid portion of the sample, even though a piston arrangement was in place to keep the ampoule filled. In preparations for the next flight of the MEPHISTO furnace an animated computer program, called MEPHISTO Volume Visualizer (MVV), was written to help avoid the formation of unwanted voids. A piston system on MEPHISTO has the ability to move approximately 5 mm in compression, to accommodate expansion of the solid during heating; then from the completely compressed position, the piston can move up to 25 mm in towards the sample, effectively making the ampoule smaller and hopefully eliminating any voids. Due to the nature of the piston design and ampoule and sample arrangement, the piston has gotten stuck during normal directional solidification; this creates the risk of a void. To eliminate such a void, the liquid in the hot zones of the furnace can be heated, thereby expanding the liquid and consuming any void. The problem with this approach is that if the liquid is heated too much an overpressure could result, breaking the ampoule and ending the experiment catastrophically. The MVV has been found to be a useful tool in the assessment of the risks associated with the formation of a void and the additional heating of the liquid in the hot zone of this Bridgman type furnace. The MVV software will be discussed and copies available; it is written in the Delphi 2 programming language and runs under Windows 95 and NT. The strategies used in other flight experiments, such as the Isothermal Dendritic Growth Experiment, will also be presented.

deGroh, Henry C., III↗

NASA NTRS1992

A new angle on lunar ferroan-suite differentiation

Small fragments of rock found among soil particles in sample 67513 from Station 11 on the southern rim of North Ray Crater at Apollo 16 yield information regarding the mafic, ferroan rocks from which they drive. We have identified a set of particles that have distinctive trace element geochemistry and whose bulk and mineral compositions indicate a genetic relationship to one another. These include polymict as well as monomict lithologies. Igneous members range from fragments with abundant anorthite to some with abundant exsolved pigeonite and augite. Consideration of this set of rock fragments, combined with mafic ferroan clasts from large breccias and from lunar-highlands meteorites suggests that there may be separate differentiation trends within the ferroan suite which are subparallel and which are less steem in Fe-Mg vs. An fractionation that the vertical trend obtained when the entire ferroan suite is taken together. This may result from a complex magma system with isolated reservoirs or separate, independently evolving magmas. Mineral compositional and textural variations are consistent with a model set forth by Longhi and Boudreau wherein the anorthite-rich samples reflect adcumulus growth with mafic crystals forming only from trapped liquid, and the more mafic samples by anorthite and pyroxene orthocumulate development.

Jolliff, B. L.↗

NASA NTRS2009

Quick-Connect Windowed Non-Stick Penetrator Tips for Rapid Sampling

Standard penetrator sampling systems were designed in order to allow for sampling via penetrators to produce a full set of sample acquisitions including volatile liquids, fine powders, and solid fragments. A gravity harpoon sampler has been designed with a removable tip and a quick coupling. The separation allows for sample handling and eliminates sample cross-contamination. Also, this design allows for multiple use of the penetrator body, which is the largest and heaviest part of the penetrator, while allowing for multiple changes of the light-mass, penetrator tip to avoid sample cross-contamination. The penetrator tip design has been improved by adding a spring trap to retain the sample, as well as a means for connecting to a quick coupling. Quick connect tips have been demonstrated in a sample handling carousel. The penetrator was released and rewound and the tips were released into a circular platter for rotation into instrument stations. The pyro-harpoon sampler was fabricated and tested with a NASA Standard Initiator (NSI) pyrotechnic charge. Initial tests collected cryogenic ice, but removal of the small pyro-harpoon from the ice was difficult. A brass metal sheath was then fitted over the harpoon tip, and removal from the ice was greatly alleviated by leaving the sheath in the ice. Quartz windows in the tips allow direct optical and spectral imaging and gas chromatography-mass spectrometer (GCMS) pyrolysis, and were found to survive impact. All systems were successfully tested by dropping into sand and into cryogenic ice.

Sherritt, Stewart↗

NASA NTRS1978

Photoacoustic spectroscopy of condensed matter

Photoacoustic spectroscopy is a new analytical tool that provides a simple nondestructive technique for obtaining information about the electronic absorption spectrum of samples such as powders, semisolids, gels, and liquids. It can also be applied to samples which cannot be examined by conventional optical methods. Numerous applications of this technique in the field of inorganic and organic semiconductors, biology, and catalysis have been described. Among the advantages of photoacoustic spectroscopy, the signal is almost insensitive to light scattering by the sample and information can be obtained about nonradiative deactivation processes. Signal saturation, which can modify the intensity of individual absorption bands in special cases, is a drawback of the method.

Somoano, R. B.↗

NASA NTRS1993

Production of long-term global water vapor and liquid water data set using ultra-fast methods to assimilate multi-satellite and radiosonde observations

During the next decade, many programs and experiments under the Global Energy and Water Cycle Experiment (GEWEX) will utilize present day and future data sets to improve our understanding of the role of moisture in climate, and its interaction with other variables such as clouds and radiation. An important element of GEWEX will be the GEWEX Water Vapor Project (GVaP), which will eventually initiate a routine, real-time assimilation of the highest quality, global water vapor data sets including information gained from future data collection systems, both ground and space based. The comprehensive global water vapor data set being produced by METSAT Inc. uses a combination of ground-based radiosonde data, and infrared and microwave satellite retrievals. This data is needed to provide the desired foundation from which future GEWEX-related research, such as GVaP, can build. The first year of this project was designed to use a combination of the best available atmospheric moisture data including: radiosonde (balloon/acft/rocket), HIRS/MSU (TOVS) retrievals, and SSM/I retrievals, to produce a one-year, global, high resolution data set of integrated column water vapor (precipitable water) with a horizontal resolution of 1 degree, and a temporal resolution of one day. The time period of this pilot product was to be det3ermined by the availability of all the input data sets. January 1988 through December 1988 were selected. In addition, a sample of vertically integrated liquid water content (LWC) was to be produced with the same temporal and spatial parameters. This sample was to be produced over ocean areas only. Three main steps are followed to produce a merged water vapor and liquid water product. Input data from Radiosondes, TOVS, and SSMI/I is quality checked in steps one and two. Processing is done in step two to generate individual total column water vapor and liquid water data sets. The third step, and final processing task, involves merging the individual output products to produce the integrated water vapor product. A final quality control is applied to the merged data sets.

Vonderhaar, T. H.↗

NASA NTRS1973

A comparison of two transient methods of measuring thermal conductivity of particulate samples.

A comparison is made of the line source (LS) method and the differential line source (DLS) method of measuring thermal conductivity of particulate materials in vacuum. The DLS method requires more instrumentation in the measuring circuitry (an additional amplifier and a differentiating circuit), but since it does not require a stable temperature to initiate a test, it does not need a sample temperature control system. DLS tests can be taken as the temperature in the samples is rising from liquid nitrogen temperature to room temperature. This eliminates the practice of extrapolating thermal conductivity over this large temperature range. Also, the advantages of reduced test time, data reduction time, and small sample temperature rise enable the experimenter to take about 7-12 DLS tests in the time of 2 LS tests. Test data from the two methods agree very well.

Scott, R. W.↗

NASA NTRS1992

Tensile properties of cast titanium alloys: Titanium-6Al-4V ELI and Titanium-5Al-2.5Sn ELI

This work was performed to determine the tensile properties of cast, hot isostatic pressed (HIP'ed), and annealed titanium alloys, Ti-6Al-4V ELI and Ti-5Al-2.5Sn ELI, that are candidate materials for the space transportation main engine (STME) liquid hydrogen turbopump impeller. Samples of the cast alloys were HIP'ed, annealed, and machined into tensile specimens. The specimens were tested in air at ambient temperature (70 F) and also at -423 F in liquid hydrogen. The Ti-6Al-4V alloy had an average ultimate strength of 129.1 ksi at 70 F and 212.2 ksi at -423 F. The Ti-5Al-2.5Sn alloy had an average ultimate strength of 108.4 ksi at 70 degrees F and 185.0 ksi at -423 F. The ductility, as measured by reduction of area, for the Ti-6Al-4V averaged 15.2 percent at 70 F and 8.7 percent at -423 F, whereas for the Ti-5Al-2.5Sn alloy average reduction of area was 24.6 percent at 70 F and 11.7 percent at -423 F.

Billinghurst, E. E., Jr.↗

NASA NTRS1999

Material Science Experiments on Mir

This paper describes the microgravity materials experiments carried out on the Shuttle/Mir program. There were six experiments, all of which investigated some aspect of diffusivity in liquid melts. The Liquid Metal Diffusion (LMD) experiment investigated the diffusivity of molten Indium samples at 185 C using a radioactive tracer, In-114m. By monitoring two different gamma ray energies (190 keV and 24 keV) emitted by the samples it was possible to measure independently the diffusion rates in the bulk and at the surface of the samples. The Queens University Experiment in Liquid Diffusion (QUELD) was the furnace facility used to process 213 samples for the five other experiments. These experiments investigated the diffusion, ripening, crystal growth, and glass formation in metal, semiconductor, and glass samples. This facility had the capability to process samples in an isothermal or gradient configuration for varying periods of time at temperatures up to 900 C. Both the LMD and the QUELD furnaces were mounted on the Microgravity Isolation Mount (MIM) which provided isolation from g-jitter. All the microgravity experiments were supported by the Space Acceleration Measurement System (SAMS); a three head three axes acceleration monitoring system which measured and recorded the acceleration environment.

Kroes, Roger L.↗

NASA NTRS1990

An eight-month sample of marine stratocumulus cloud fraction, albedo, and integrated liquid water

Surface-meteorology and shortwave/longwave irradiance measurements taken on the northwest tip of San Nicolas Island off the coast of Southern California from March through October 1987 are analyzed. Experimental details are summarized, and shortwave cloud-radiation parameterization is outlined with emphasis on a shortwave algorithm. Frequency distributions indicate the stratocumulus clouds at the island have a cloud base on the order of 400 m, an integrated liquid water content of 75 g/sq m, and an albedo of 0.55 with substantial diurnal variations. The longwave parameterization for cloud fraction is also considered, and it is noted that using these models for downward longwave and shortwave irradiances, cloud fraction, integrated liquid water content, and albedo are deduced from the data.

Fairall, C. W.↗

NASA NTRS2003

Early Petrologic Processes on the Ureilite Parent Body

We present a petrographic and petrologic analysis of 21 olivine-pigeonite ureilites, along with new experimental results on melt compositions predicted to be in equilibrium with ureilite compositions. We conclude that these ureilites are the residues of a partial melting/smelting event. Textural evidence preserved in olivine and pigeonite record the extent of primary smelting. In pigeonite cores, we observe fine trains of iron metal inclusions that formed by the reduction of olivine to pigeonite and metal during primary smelting. Olivine cores lack metal inclusions but the outer grain boundaries are variably reduced by a late-stage reduction event. The modal proportion of pigeonite and percentage of olivine affected by late stage reduction are inversely related and provide an estimation of the degree of primary smelting during ureilite petrogenesis. In our sample suite, this correlation holds for 16 of the 21 samples examined. Olivine-pigeonite-liquid phase equilibrium constraints are used to obtain temperature estimates for the ureilite samples examined. Inferred smelting temperatures range from approximately 1150 C to just over 1300 C and span the range of estimates published for ureilites containing two or more pyroxenes. Temperature is also positively correlated with modal percent pigeonite. Smelting temperature is inversely correlated with smelting depth--the hottest olivine-pigeonite ureilites coming from the shallowest depth in the ureilite parent body. The highest temperature samples also have oxygen isotopic signatures that fall toward the refractory inclusion-rich end of the carbonaceous chondrite-anhydrous mineral (CCAM) slope 1 mixing line. These temperature-depth variations in the ureilite parent body could have been created by a heterogeneous distribution of heat producing elements, which would indicate that isotopic heterogeneities existed in the material from which the ureilite parent body was assembled.

Singletary, S. J.↗

NASA NTRS2023

Solidification Furnace for In Situ Observation of Bulk Transparent Systems and Image Analysis Methods

This paper aims to describe the experimental framework of the Directional Solidification Insert (DSI), installed onboard the International Space Station (ISS), dedicated to the in situ and real-time characterization of the dynamic selection of the solid-liquid interface morphology in bulk samples of transparent materials under diffusive growth conditions. The in situ observation of the solid-liquid interface is an invaluable tool for gaining knowledge on the time-evolution of the interface pattern because the initial morphological instability evolves nonlinearly and undergoes a reorganization process. The result of each experiment, characterized by the sample concentration, a thermal gradient and a pulling rate, is a large number of images. Interpretation of these images necessitates a robust identification of each cell/dendrite position and size during the entire solidification. Several image analysis methods have been developed to achieve this goal reliably despite varying contrast and noise levels, and are described in details. Typical solidification experiments are presented and the dynamics of the pattern formation are analyzed to illustrate the application of the image analysis methods.

Programming languages↗

NASA NTRS2014

Warm Pressurant Gas Effects on the Static Bubble Point Pressure for Cryogenic LADs

This paper presents experimental results for the liquid hydrogen and nitrogen bubble point tests using warm pressurant gases conducted at the NASA Glenn Research Center. The purpose of the test series was to determine the effect of elevating the temperature of the pressurant gas on the performance of a liquid acquisition device (LAD). Three fine mesh screen samples (325x2300, 450x2750, 510x3600) were tested in liquid hydrogen and liquid nitrogen using cold and warm non-condensable (gaseous helium) and condensable (gaseous hydrogen or nitrogen) pressurization schemes. Gases were conditioned from 0K - 90K above the liquid temperature. Results clearly indicate degradation in bubble point pressure using warm gas, with a greater reduction in performance using condensable over non-condensable pressurization. Degradation in the bubble point pressure is inversely proportional to screen porosity, as the coarsest mesh demonstrated the highest degradation. Results here have implication on both pressurization and LAD system design for all future cryogenic propulsion systems. A detailed review of historical heated gas tests is also presented for comparison to current results.

Warm pressurant gas↗

NASA NTRS2011

Sample Acquisition and Handling System from a Remote Platform

A system has been developed to acquire and handle samples from a suspended remote platform. The system includes a penetrator, a penetrator deployment mechanism, and a sample handler. A gravity-driven harpoon sampler was used for the system, but other solutions can be used to supply the penetration energy, such as pyrotechnic, pressurized gas, or springs. The deployment mechanism includes a line that is attached to the penetrator, a spool for reeling in the line, and a line engagement control mechanism. The penetrator has removable tips that can collect liquid, ice, or solid samples. The handling mechanism consists of a carousel that can store a series of identical or different tips, assist in penetrator reconfiguration for multiple sample acquisition, and deliver the sample to a series of instruments for analysis. The carousel sample handling system was combined with a brassboard reeling mechanism and a penetrator with removable tips. It can attach the removable tip to the penetrator, release and retrieve the penetrator, remove the tip, and present it to multiple instrument stations. The penetrator can be remotely deployed from an aerobot, penetrate and collect the sample, and be retrieved with the sample to the aerobot. The penetrator with removable tips includes sample interrogation windows and a sample retainment spring for unconsolidated samples. The line engagement motor can be used to control the penetrator release and reeling engagement, and to evenly distribute the line on the spool by rocking between left and right ends of the spool. When the arm with the guiding ring is aligned with the spool axis, the line is free to unwind from the spool without rotating the spool. When the arm is perpendicular to the spool axis, the line can move only if the spool rotates.

Badescu, Mircea↗

NASA NTRSDate not supplied

Test Results for the SEA Ice Crystal Detector (ICD) under SLD Conditions at the NASA IRT

The Science Engineering Associates hot-wire Ice Crystal Detector was tested under Appendix C and Supercooled Large Drop Conditions at the NASA Icing Research Tunnel, with the purpose of comparing the measurements to the tunnel LWC calibration, and to test the performance of the mixed-phase retrievals of the probe. The liquid water content measured by the total water content sensor of the probe agreed well with the tunnel calibration over a wide range of MVDs, not unexpectedly since the tunnel was calibrated with a similar Multiwire hot-wire probe. A scale factor difference of about 7% was attributed to the lack of an efficiency correction for the Ice Crystal Detector at smaller median volume diameters, and typical sample area uncertainties of liquid water content devices. In addition, the simultaneous equations that are used to retrieve liquid and ice water contents were tested under liquid and glaciated conditions. Using constant ice and water efficiencies for each wire, the equations were found to produce a large and false ice water content retrieval in large median volume diameter liquid cases. By applying a liquid efficiency to the liquid water content sensor that varied with median volume diameter, retrievals were improved such that false ice water content was less than ±10% of the total water content out to the 460 μm median volume diameter limit of the testing. The probe was also tested in glaciated conditions by freezing out a small median volume diameter spray. Using constant ice efficiencies for the two sensors provided from aircraft measurements, the retrieved ice water content was about 40% higher than expected for the case presented, likely due to the ice efficiencies that were used from aircraft measurements of natural clouds being too low for the tunnel’s glaciated sprays. Application of ice efficiencies that vary with particle size and potentially other parameters will be explored for future improvement of retrievals.

Air Craft Icing↗