A simple combination mass spectrometer inlet and oxygen electrode chamber for sampling gases dissolved in liquids.
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Stuart, T. S.↗
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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.
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Temperature Dependence of Diffusivities in Liquid Elements (LMD)
This research was to advance the understanding of diffusion mechanisms in liquid metals and alloys through accurate diffusivity measurements over a wide range of temperatures, including the proximity of the materials melting points. Specifically, it was driven towards developing a methodology (and subsequent flight hardware) to enable several diffusion coefficient measurements (i.e., at several different temperatures) to be performed using a single sample. The Liquid Metal Diffusion (LMD) was funded as a Flight Definition Project in February 1993 in response to NRA 91-OSSA-20 (Microgravity Science and Applications Division). The Science Concept Review for LAID was held during April 1994. In January 1995 we were informed that we had failed this review and the project was change to ground-based activities only. A new proposal was submitted for the next NRA addressing the panels concerns. As part of NASA's Risk Mitigation program, a scaled-down version of the hardware was funded in July of 1995 for a flight opportunity utilizing experiment on the Microgravity Isolation Mount. This experiment was to determine the self-diffusivity of indium at 185 C. The LMD was transferred to the Mir Space Station in STS-81 and returned on STS-84 (January - May 1997). Three, out of five, self-diffusion data sets were returned. A description of this experiment/hardware is included below. This summary is only intended to give the reader an overview of the results obtained for the tasks outlined in the original proposal. Research that was not published is explained in more detail. At the end of this report is a list of refereed publications and invited talks that were given as a result of this work. The reader is directed to these for further details. Attachment: Real-time diffusivity measurements in liquids at several temperatures with one sample, On the insensitivity of liquid diffusivity measurements to deviations from 1D transport, and Numerical simulations of the convective contamination of diffusivity measurements in liquids.
Banish, R. Michael↗
Technique for Performing Dielectric Property Measurements at Microwave Frequencies
A paper discusses the need to perform accurate dielectric property measurements on larger sized samples, particularly liquids at microwave frequencies. These types of measurements cannot be obtained using conventional cavity perturbation methods, particularly for liquids or powdered or granulated solids that require a surrounding container. To solve this problem, a model has been developed for the resonant frequency and quality factor of a cylindrical microwave cavity containing concentric cylindrical samples. This model can then be inverted to obtain the real and imaginary dielectric constants of the material of interest. This approach is based on using exact solutions to Maxwell s equations for the resonant properties of a cylindrical microwave cavity and also using the effective electrical conductivity of the cavity walls that is estimated from the measured empty cavity quality factor. This new approach calculates the complex resonant frequency and associated electromagnetic fields for a cylindrical microwave cavity with lossy walls that is loaded with concentric, axially aligned, lossy dielectric cylindrical samples. In this approach, the calculated complex resonant frequency, consisting of real and imaginary parts, is related to the experimentally measured quantities. Because this approach uses Maxwell's equations to determine the perturbed electromagnetic fields in the cavity with the material(s) inserted, one can calculate the expected wall losses using the fields for the loaded cavity rather than just depending on the value of the fields obtained from the empty cavity quality factor. These additional calculations provide a more accurate determination of the complex dielectric constant of the material being studied. The improved approach will be particularly important when working with larger samples or samples with larger dielectric constants that will further perturb the cavity electromagnetic fields. Also, this approach enables the ability to have a larger sample of interest, such as a liquid or powdered or granulated solid, inside a cylindrical container.
Barmatz, Martin B.↗
Pseudo continuous wave instrument
Acoustic properties and their changes in a sample of liquid, gas, plasma or solid are measured by applying a variable frequency source to the sample by means of a transducer to produce sound waves within the sample. The application of the variable frequency source to the sample is periodically interrupted for a short duration. Means are connected to the transducer for receiving the resulting acoustic signals during the interruptions for producing a control signal indicative of a difference in the frequency of the output of the variable frequency source and the frequency of a mechanical resonant peak in the sample. The control signal is applied to the variable frequency source to maintain its output frequency at the frequency of the mechanical resonant peak. The change in frequency of the variable frequency source indicates the shift in frequency of the mechanical resonant peak and the amplitude of the acoustic signals indicates the attenuation of the acoustic signals in the sample.
Heyman, J. S.↗
Containerless processing technologies at the Jet Propulsion Laboratory
Acoustic and electrostatic levitation (EL) techniques for maintaining sample-wall distance in order to ensure contamination-free conditions during microgravity materials science experiments on board the Shuttle are examined. A laboratory model for acoustic containerless (AC) processing is described, noting the use of three commercially available drivers for sample levitation. The arrangement of the speakers results in a point node to which a liquid drop sample migrates. Varying the field through manipulation of the dB levels and phase of the drivers' outputs permits control of sample position and movement. Rotation of a styrofoam ball at 2000 rpm has been achieved. Oscillations can also be induced. An advanced version of the AC system is analytically defined, with further studies mentioned for stable levitation modes using a cylindrical chamber and optimizing acoustic power transfer between hot and cold regions. A tetrahedral EL system has proven to work in a reduced gravity environment. El involves imparting an electrical charge to an object and then positioning and maintaining it through use of EM fields. The presence of human operators to perform the processing on the Shuttle is mentioned as offering real-time capability of altering the experimental conditions.
Wang, T. G.↗
Lunar Science Conference, 5th, Houston, Tex., March 18-22, 1974, Proceedings. Volume 1 - Mineralogy and petrology. Volume 2 Chemical and isotope analyses. Organic chemistry. Volume 3 - Physical properties
Numerous studies on the properties of the moon based on Apollo findings and samples are presented. Topics treated include ages of the lunar nearside light plains and maria, orange material in the Sulpicius Gallus formation at the southwestern edge of Mare Serenitatis, impact-induced fractionation in the lunar highlands, igneous rocks from Apollo 16 rake samples, experimental liquid line of descent and liquid immiscibility for basalt 70017, ion microprobe mass analysis of plagioclase from 'non-mare' lunar samples, grain size and the evolution of lunar soils, chemical composition of rocks and soils at Taurus-Littrow, the geochemical evolution of the moon, U-Th-Pb systematics of some Apollo 17 lunar samples and implications for a lunar basin excavation chronology, volatile-element systematics and green glass in Apollo 15 lunar soils, solar wind nitrogen and indigenous nitrogen in Apollo 17 lunar samples, lunar trapped xenon, solar flare and lunar surface process characterization at the Apollo 17 site, and the permanent and induced magnetic dipole moment of the moon. Individual items are announced in this issue.
Gose, W. A.↗
Plasma-Based Elemental Analyzer for Crewed Transit and Planetary Habitation
As NASA continues to perform research on the ISS and move towards the Moon and Mars, it is important for astronauts to have a technology capable of determining the composition of solid, liquid, and gas samples. Currently, samples are transported back to Earth for analysis, which may impact results due to the time delay of samples waiting to be returned to Earth as well as potential sample contamination from re-entry, change in environment, and various personnel handling. Therefore, researchers at the Applied Chemistry Lab at KSC have developed a proof-of-concept “Plasma-Based Elemental Analyzer,” which has the capability of testing solid, liquid, and gas samples for identification. Currently, the analysis is only qualitative, with quantitative identification left for future work. This technology is similar to ICP-OES, but differs in instrument size and sample preparation. Both technologies use plasma to ionize samples for light emission. The plasma elemental analyzer aims to be portable and lightweight, require only electrical power, and analyze solid, liquid, and gas samples. It does not use acid digestion or a nebulizer, requires less power than ICP-OES, and is able to operate with minimal to no usage of argon gas. Furthermore, the plasma elemental analyzer operates within low power constraints, which makes it feasible for usage on future missions with higher power constraints. The technology was tested at atmospheric pressure using mostly room air as the carrier gas for plasma production in the proof-of-concept study. The results showed the peak signals of the elements with an associated arbitrary signal intensity that allowed for qualitative identification. Solid samples that were tested included inedible biomass from the Golden Heirloom Cherry Tomato plant and Lunar Highlands Simulants (LHS-1). The liquid samples included elements of interest for the space crop production community. This work showed that a system smaller than the traditional ICP-OES equipment is able to be designed and implemented in future use cases, although it requires further development.
Kenneth Engeling↗
Evaluation of analytical methodology for hydrocarbons in high pressure air and nitrogen systems
Samples of liquid oxygen, high pressure nitrogen, low pressure nitrogen, and missile grade air were studied to determine the hydrocarbon concentrations. Concentration of the samples was achieved by adsorption on a molecular sieve and activated charcoal. The trapped hydrocarbons were then desorbed and transferred to an analytical column in a gas chromatograph. The sensitivity of the method depends on the volume of gas passed through the adsorbent tubes. The value of the method was verified through recoverability and reproducibility studies. The use of this method enables LOX, GN2, and missile grade air systems to be routinely monitored to determine low level increases in specific hydrocarbon concentration that could lead to potentially hazardous conditions.
Source record↗
Marangoni-Benard Convection in a Evaporating Liquid Thin Layer
Marangoni-Benard convection in evaporating liquid thin layers has been investigated through flow visualization and temperature profile measurement. Twelve liquids, namely ethyl alcohol, methanol, chloroform, acetone, cyclohexane, benzine, methylene chloride, carbon tetrachloride, ethyl acetate, n-pentane, silicone oil (0.65 cSt.), and freon-113, were tested and convection patterns in thin layers of these samples were observed. Comparison among these tested samples shows that some liquids are sensitive to surface contamination from aluminum powder but some are not. The latter is excellent to be used for the investigation of surface-tension driven convection through visualization using the tracer. Two sample liquids, alcohol and freon-113 were particularly selected for systematic study. It was found that the wavelength of Benard cells would not change with thickness of the layer when it evaporates at room temperature. Special attention was focused on cases in which a liquid layer was cooled from below, and some interesting results were obtained. Convection patterns were recorded during the evaporation process and the patterns at certain time frame were compared. Benard cells were observed in thin layers with a nonlinear temperature profile and even with a zero or positive temperature gradient. Wavelength of the cells was found to increase as the evaporation progressed.
Chai, An-Ti↗
Analysis of Mars Analogue Soil Samples Using Solid-Phase Microextraction, Organic Solvent Extraction and Gas Chromatography/Mass Spectrometry
Polycyclic aromatic hydrocarbons (PAHs) are robust and abundant molecules in extraterrestrial environments. They are found ubiquitously in the interstellar medium and have been identified in extracts of meteorites collected on Earth. PAHs are important target molecules for planetary exploration missions that investigate the organic inventory of planets, moons and small bodies. This study is part of an interdisciplinary preparation phase to search for organic molecules and life on Mars. We have investigated PAH compounds in desert soils to determine their composition, distribution and stability. Soil samples (Mars analogue soils) were collected at desert areas of Utah in the vicinity of the Mars Desert Research Station (MDRS), in the Arequipa region in Peru and from the Jutland region of Denmark. The aim of this study was to optimize the solid-phase microextraction (SPME) method for fast screening and determination of PAHs in soil samples. This method minimizes sample handling and preserves the chemical integrity of the sample. Complementary liquid extraction was used to obtain information on five- and six-ring PAH compounds. The measured concentrations of PAHs are, in general, very low, ranging from 1 to 60 ng g(sup -1). The texture of soils is mostly sandy loam with few samples being 100% silt. Collected soils are moderately basic with pH values of 8-9 except for the Salten Skov soil, which is slightly acidic. Although the diverse and variable microbial populations of the samples at the sample sites might have affected the levels and variety of PAHs detected, SPME appears to be a rapid, viable field sampling technique with implications for use on planetary missions.
Orzechowska, G. E.↗
Acoustic containerless experiment system: A non-contact surface tension measurement
The Acoustic Containerless Experiment System (ACES) was flown on STS 41-B in February 1984 and was scheduled to be reflown in 1986. The primary experiment that was to be conducted with the ACES module was the containerless melting and processing of a fluoride glass sample. A second experiment that was to be conducted was the verification of a non-contact surface tension measurement technique using the molten glass sample. The ACES module consisted of a three-axis acoustic positioning module that was inside an electric furnace capable of heating the system above the melting temperature of the sample. The acoustic module is able to hold the sample with acoustic forces in the center of the chamber and, in addition, has the capability of applying a modulating force on the sample along one axis of the chamber so that the molten sample or liquid drop could be driven into one of its normal oscillation modes. The acoustic module could also be adjusted so that it could place a torque on the molten drop and cause the drop to rotate. In the ACES, a modulating frequency was applied to the drop and swept through a range of frequencies that would include the n = 2 mode. A maximum amplitude of the drop oscillation would indicate when resonance was reached and from that data the surface tension could be calculated. For large viscosity samples, a second technique for measuring surface tension was developed. The results of the ACES experiment and some of the problems encountered during the actual flight of the experiment will be discussed.
Elleman, D. D.↗
Determination of (alpha)-dialkylamino acids and their Enantiomers in Geological Samples by High-Performance Liquid Chromatography after Dervatization with a Chiral Adduct of (omicron)-Phthaldialdehyde
Derivatization with (omicron)-phthaldialdehyde (OPA) and the chiral thiol N-acetyl-L-cysteine (NAC) is a convenient and sensitive technique for the HPLC detection and resolution of protein amino acid enantiomers. The kinetics of the reaction of OPA-NAC with (alpha)-dialkylamino acids was investigated. The fluorescence yield of (alpha)-dialkylamino acids was only about 10% of that of protein amino acids when the derivatization was carried out at room temperature for 1-2 min, which is the procedure generally used for protein amino acid analyses. The fluorescence yield of (alpha)-dialkylamino acids can be enhanced by up to ten-fold when the derivatization reaction time is increased to 15 min at room temperature. The OPA-NAC technique was optimized for the detection and enantiomeric resolution of a-dialkylamino acids in geological samples which contain a large excess of protein amino acids. The estimated detection limit for a-dialkylamino acids is 1-2 pmol, comparable to that for protein amino acids.
Zhoa, Meixun↗
Liquid Metering Centrifuge Sticks (LMCS): A Centrifugal Approach to Metering Known Sample Volumes for Colorimetric Solid Phase Extraction (C-SPE)
Phase separation is one of the most significant obstacles encountered during the development of analytical methods for water quality monitoring in spacecraft environments. Removing air bubbles from water samples prior to analysis is a routine task on earth; however, in the absence of gravity, this routine task becomes extremely difficult. This paper details the development and initial ground testing of liquid metering centrifuge sticks (LMCS), devices designed to collect and meter a known volume of bubble-free water in microgravity. The LMCS uses centrifugal force to eliminate entrapped air and reproducibly meter liquid sample volumes for analysis with Colorimetric Solid Phase Extraction (C-SPE). C-SPE is a sorption-spectrophotometric platform that is being developed as a potential spacecraft water quality monitoring system. C-SPE utilizes solid phase extraction membranes impregnated with analyte-specific colorimetric reagents to concentrate and complex target analytes in spacecraft water samples. The mass of analyte extracted from the water sample is determined using diffuse reflectance (DR) data collected from the membrane surface and an analyte-specific calibration curve. The analyte concentration can then be calculated from the mass of extracted analyte and the volume of the sample analyzed. Previous flight experiments conducted in microgravity conditions aboard the NASA KC-135 aircraft demonstrated that the inability to collect and meter a known volume of water using a syringe was a limiting factor in the accuracy of C-SPE measurements. Herein, results obtained from ground based C-SPE experiments using ionic silver as a test analyte and either the LMCS or syringes for sample metering are compared to evaluate the performance of the LMCS. These results indicate very good agreement between the two sample metering methods and clearly illustrate the potential of utilizing centrifugal forces to achieve phase separation and metering of water samples in microgravity.
Gazda, Daniel B.↗
Hydrogen Fire in a Storage Vessel
On October 23, 2007, the operations team began a procedure to sample the Liquid Hydrogen (LH2) storage vessels ("tanks"), and associated transfer system. This procedure was being performed to determine the conditions within the system, and if necessary, to purge the system of any excess Gaseous Hydrogen (GH2) in preparation for reactivation of the system. The system had not been used since 2003. The LH2 storage system contains two (2) spherical pressure vessels of 225,000 gallons in volume, with a maximum working pressure (MAWP) of 50 psig. Eight inch transfer piping connects them to the usage point. Operations began with activation of the burnstack for the LH2 storage area. Pneumatic (GN2) systems in the storage area were then activated and checked. Pressurization of storage tank number 1 with gaseous nitrogen (GN2) was initiated, with a target pressure of 10 psig, at which point samples were planned to be taken. At 5 psig, a loud noise was heard in the upper area of tank number 2. Smoke was seen exiting the burnstack and from the insulation on vent lines for both tanks. At this time tank number 1 was vented and the pressurization system was secured. The mishap resulted in physical damage to both storage tanks, as well as to some of the piping for both tanks. Corrective action included repair of the damaged hardware by a qualified contractor. Preventive action included documented organizational policy and procedures for establishing standby and mothball conditions for facilities and equipment, including provisions as detailed in the investigation report recommendations: Recommendation 1: The using organization should define necessary activities in order to place hydrogen systems in long term periods of inactivity. The defined activities should address requirements for rendering inert, isolation (i.e., physical disconnect, double block and bleed, etc.) and periodic monitoring. Recommendation 2: The using organization should develop a process to periodically monitor hazardous systems for proper configuration (i.e., a daily/weekly/monthly check sheet to verify critical purges are active).
Hester, Zena M.↗
OASIS: Organics Analyzer for Sampling Icy Surfaces
Liquid chromatography mass spectrometry (LC-MS) is a well established laboratory technique for detecting and analyzing organic molecules. This approach has been especially fruitful in the analysis of nucleobases, amino acids, and establishing chirol ratios [1 -3]. We are developing OASIS, Organics Analyzer for Sampling Icy Surfaces, for future in situ landed missions to astrochemically important icy bodies, such as asteroids, comets, and icy moons. The OASIS design employs a microfabricated, on-chip analytical column to chromatographically separate liquid ana1ytes using known LC stationary phase chemistries. The elution products are then interfaced through electrospray ionization (ESI) and analyzed by a time-of-flight mass spectrometer (TOF-MS). A particular advantage of this design is its suitability for microgravity environments, such as for a primitive small body.
Getty, S. A.↗
Eutectic superalloys by edge-defined, film-fed growth
The feasibility of producing directionally solidified eutectic alloy composites by edge-defined, film-fed growth (EFG) was carried out. The three eutectic alloys which were investigated were gamma + delta, gamma/gamma prime + delta, and a Co-base TaC alloy containing Cr and Ni. Investigations into the compatibility and wettability of these metals with various carbides, borides, nitrides, and oxides disclosed that compounds with the largest (negative) heats of formation were most stable but poorest wetting. Nitrides and carbides had suitable stability and low contact angles but capillary rise was observed only with carbides. Oxides would not give capillary rise but would probably fulfill the other wetting requirements of EFG. Tantalum carbide was selected for most of the experimental portion of the program based on its exhibiting spontaneous capillary rise and satisfactory slow rate of degradation in the liquid metals. Samples of all three alloys were grown by EFG with the major experimental effort restricted to gamma + delta and gamma/gamma prime + delta alloys. In the standard, uncooled EFG apparatus, the thermal gradient was inferred from the growth speed and was 150 to 200 C/cm. This value may be compared to typical gradients of less than 100 C/cm normally achieved in a standard Bridgman-type apparatus. When a stream of helium was directed against the side of the bar during growth, the gradient was found to improve to about 250 C/cm. In comparison, a theoretical gradient of 700 C/cm should be possible under ideal conditions, without the use of chills. Methods for optimizing the gradient in EFG are discussed, and should allow attainment of close to the theoretical for a particular configuration.
Hurley, G. F.↗
Helium-4 Experiments near T-lambda in a Low-Gravity Simulator
We report our studies of gravity cancellation in a liquid helium sample cell along the lambda-line using a low-gravity simulator facility. The simulator consists of a superconducting magnet capable of producing B(delta-B/delta-z) = 22squareT)/cm. We have verified experimentally that the simulator can cancel gravity to about 0.01g in a cylindrical sample volume of 0.5 cm in diameter and 0.5 cm in height. This allows us to approach more closely the superfluid transition without entering the normal-superfluid two phase region induced by gravity. We also present the measurements of T-c(Q,P): depression of the superfluid transition temperature by a heat current(Q) along the lambda-line (P). The results are consistent with the Renormalization-group theory calculation. Measurements of thermal expansion coefficient in a heat current will also be discussed. The work has been carried out by JPL, California Institute of Technology under contract to NASA.
Liu, Yuanming↗
A Theoretical Light Scattering Model of Nanoparticle Laser Tweezers
Accomplishments this reporting period include: 1. derived, programmed, checked, and tested the Mie light scattering theory formulas for the radiation trapping force for both the on-axis and off-axis geometry of the trapping beam plus trapped spherical particle; 2. verified that the computed radiation trapping force for a freely propagating focused Gaussian laser beam incident on a spherical particle agrees with previous published calculations; 3. compared the small particle size and large particle size limits of the Mie calculation with the results of Rayleigh scattering theory and ray scattering theory, respectively and verified that the comparison is correct for Rayleigh scattering theory but found that ray theory omits an important light scattering effect included in the Mie theory treatment; 4. generalized the calculation of the radiation trapping force on a spherical particle in the on-axis geometry from a freely propagating focused Gaussian laser beam to the realistic situation of a Gaussian beam truncated and focused by a high numerical aperture oil-immersion microscope objective lens and aberrated by the interface between the microscope cover slip and the liquid-filled sample volume; and 5. compared the calculated radiation trapping force for this geometry with the results of previously published experiments and found that the agreement is better than when using previously developed theories.
Lock, James A.↗