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Small portable pumping station, consisting of roughing pump, air cooled diffusion pump, and liquid nitrogen cold trap, permits onsite sampling followed by quantitative laboratory analysis of residual gases.
Flowing-liquid cleaner may be used to gently dislodge and remove 98 percent of biological particulates from surfaces. Cleaner may retain up to 90 percent of removed particulates for later analysis. If retention is not required, unit may be adapted to clean only. Cleaner is applicable wherever very clean surface is desired.
The Diviner Lunar Radiometer, onboard NASA's Lunar Reconnaissance Orbiter, has produced the first global, high resolution, thermal infrared observations of an airless body. The Moon, which is the most accessible member of this most abundant class of solar system objects, is also the only body for which we have extraterrestrial samples with known spatial context, returned Apollo samples. Here we present the results of a comprehensive study to reproduce an accurate simulated lunar environment, evaluate the most appropriate sample and measurement conditions, collect thermal infrared spectra of a representative suite of Apollo soils, and correlate them with Diviner observations of the lunar surface. It has been established previously that thermal infrared spectra measured in simulated lunar environment (SLE) are significantly altered from spectra measured under terrestrial or martian conditions. The data presented here were collected at the University of Oxford Simulated Lunar Environment Chamber (SLEC). In SLEC, we simulate the lunar environment by: (1) pumping the chamber to vacuum pressures (less than 10‐4 mbar) sufficient to simulate lunar heat transport processes within the sample, (2) cooling the chamber with liquid nitrogen to simulate radiation to the cold space environment, and (3) heating the samples with heaters and lamp to set‐up thermal gradients similar to those experienced in the upper hundreds of microns of the lunar surface. We then conducted a comprehensive suite of experiments using different sample preparation and heating conditions on Apollo soils 15071 (maria) and 67701 (highland) and compared the results to Diviner noontime data to select the optimal experimental conditions. This study includes thermal infrared SLE measurements of 10084 (A11 - LM), 12001 (A12 - LM), 14259 (A14 - LM), 15071 (A15 - S1), 15601 (A15 - S9a), 61141 (A16 - S1), 66031 (A16 - S6), 67701 (A16 - S11), and 70181 (A17 - LM). The Diviner dataset includes all six Apollo sites at approximately 200 m spatial resolution We find that analyses of Diviner observations of individual sampling stations and SLE measurements returned Apollo soils show good agreement, while comparisons to thermal infrared reflectance under ambient conditions do not agree well, which underscores the need for SLE measurements and validates the Diviner compositional measurement technique.
The atomic force microscope (AFM) is used to inject a sample, provide shear-driven liquid flow over a functionalized substrate, and detect separated components. This is demonstrated using lipophilic dyes and normal phase chromatography. A significant reduction in both size and separation time scales is achieved with a 25-micron-length column scale, and one-second separation times. The approach has general applications to trace chemical and microfluidic analysis. The AFM is now a common tool for ultra-microscopy and nanotechnology. It has also been demonstrated to provide a number of microfluidic functions necessary for miniaturized chromatography. These include injection of sub-femtoliter samples, fluidic switching, and sheardriven pumping. The AFM probe tip can be used to selectively remove surface layers for subsequent microchemical analysis using infrared and tip-enhanced Raman spectroscopy. With its ability to image individual atoms, the AFM is a remarkably sensitive detector that can be used to detect separated components. These diverse functional components of microfluidic manipulation have been combined in this work to demonstrate AFM mediated chromatography. AFM mediated chromatography uses channel-less, shear-driven pumping. This is demonstrated with a thin, aluminum oxide substrate and a non-polar solvent system to separate a mixture of lipophilic dyes. In conventional chromatographic terms, this is analogous to thin-layer chromatography using normal phase alumina substrate with sheardriven pumping provided by the AFM tip-cantilever mechanism. The AFM detection of separated components is accomplished by exploiting the variation in the localized friction of the separated components. The AFM tip-cantilever provides the mechanism for producing shear-induced flows and rapid pumping. Shear-driven chromatography (SDC) is a relatively new concept that overcomes the speed and miniaturization limitations of conventional liquid chromatography. SDC is based on a sliding plate system, consisting of two flat surfaces, one of which has a recessed channel. A fluid flow is produced by axially sliding one plate past another, where the fluid has mechanical shear forces imposed at each point along the channel length. The shear-induced flow rates are very reproducible, and do not have pressure or voltage gradient limitations. SDC opens up a new range of enhanced separation kinetics by permitting the sample confinement with submicron dimensions. Small, highly confined liquid is advantageous for chromatographic separation because the separation rate is known to scale according to the square of the confined sample diameter. In addition, because shear-driven flows are not limited by fluid velocity, shear-driven liquid chromatography may provide up to 100,000 plate efficiency.
The Mars Exploration Rover Spirit has traversed over 7.5 km in 1470 sols of operations at the Gusev Crater landing site. Chemical and mineralogical evidence from approximately 200 in-situ samples indicate various degrees of exposure to liquid water, from wet and saturated to dry and unaltered. (1) Six samples with concentrations of amorphous silica between 60 and 95 wt% were discovered in a small valley less than 50 meters in length. Associated enrichments in titanium oxide, relatively insoluble at low pH, suggest that these silica deposits formed as a result of acidic leaching processes. Liquid water interactions with these surface materials were necessary to remove cations solubilized in the low pH environment or to concentrate silica in solution prior to precipitation. (2) Hydrated ferric sulfates are found in subsurface deposits which have the unmistakable chemical signatures of nearby rocks. The movement of hydrothermal fluids and/or fumarolic vapors through local rocks prior to precipitation of these materials is suggested by these observations. (3) Goethite (alpha-FeOOH), a mineral phase which requires water to form, represents 20% to 35% of the iron in numerous rock samples (Clovis Class) on the West Spur of the Columbia Hills. Alteration of iron under aqueous conditions is clearly indicated by this presence of goethite. (4) Nearly isochemical signatures are found in elemental analyses of over ten distinct samples (Wishstone/Watchtower class rocks), yet the ratio of ferric iron to total iron varies from 0.4 to 0.95. Small quantities of water, insufficient to flush cations from the samples, were likely responsible for this weathering. (5) Bromine, a trace element readily mobilized by water, is found in high concentrations in certain rock interiors and is enhanced in subsurface soils, consistent with transport to localized cold traps by water thin-films. (6) Also relevant to the characterizing the role of liquid water is the discovery of an areally extensive ultramafic sequence of rocks where over 70% of the iron is in unaltered olivine and the ferric to total iron ratio is 0.1. This result indicates that certain materials at the martian surface have been protected from aqueous alteration.
ZrB2 - 20v% SiC - 20v% TaSi2 was oxidized in stagnant air for ten minute cycles for times up to 100 minutes at 1627 C and 1927 C. The sample oxidized at 1627 C showed oxidation resistance better than that of the standard ZrB2 - 20v% SiC. The sample oxidized at 1927 C, however, showed evidence of liquid phase formation and complex oxidation products. The sample exposed at 1927 C was analyzed in detail by scanning electron microprobe and wavelength dispersive spectroscopy to understand the complex oxidation and melting reactions occurring during exposure. The as hot-pressed material shows the formation of a Zr(Ta)B2 phase in addition to the three phases in the nominal composition already noted. After oxidation, the TaSi2 in the matrix was completely reacted to form Ta(Zr)C. The layered oxidation products included SiO2, ZrO2, Ta2O5, and a complex oxide containing both Zr and Ta. Likely reactions are proposed based on thermodynamic phase stability and phase morphology.
Two phase liquid and gaseous nitrogen flow in a pneumatic two fluid atomizer was investigated. Characteristic dropsize for cryogenic sprays were measured with a scattered light scanning instrument developed at NASA-Lewis. Tests were conducted primarily in the aerodynamic stripping regime of liquid jet atomization. At a sampling distance of bar-x=1.3 cm, the Sauter mean, D(sub 32), and volume median, D(sub v.5), drop diameters were measured and correlated with nitrogen gas flowrate, W(sub n), to give the following expressions: D sub 32 to the -1=210W(sub n) to the -1.33 and D(sub v.5) to the -1=150 W(sub n to the -1.33, where reciprocal diameters and gas flowrate are in cm (-1) and g/sec, respectively. The exponent 1.33 for nitrogrn gas flowrate, W(sub n), is the same as that predicted by atomization theory for liquid-jet breakup in high velocity gasflow. When the spray was sampled at axial distances of bar-x=2.5 and 4.5 cm downstream of the atomizer, the exponent decreased to 1.2 and 0.9, respectively. This was attributed to the loss of small droplets due to their rapid vaporization.
Two phase liquid and gaseous nitrogen flow in a pneumatic two fluid atomizer was investigated. Characteristic dropsize for cryogenic sprays were measured with a scattered light scanning instrument developed at NASA-Lewis. Tests were conducted primarily in the aerodynamic stripping regime of liquid jet atomization. At a sampling distance of bar-x =1.3 cm, the Sauter mean, D(sub 32), and volume median, D(sub v.5), drop diameters were measured and correlated with nitrogen gas flowrate, W(sub n), to give the following expressions: D sub 32 to the -1=210W(sub n) to the -1.33 and D(sub v.5) to the -1=150 W(sub n to the -1.33, where reciprocal diameters and gas flowrate are in cm (-1) and g/sec, respectively. The exponent 1.33 for nitrogen gas flowrate, W(sub n), is the same as that predicted by atomization theory for liquid-jet breakup in high velocity gasflow. When the spray was sampled at axial distances of bar-x=2.5 and 4.5 cm downstream of the atomizer, the exponent decreased to 1.2 and 0.9, respectively. This was attributed to the loss of small droplets due to their rapid vaporization.
A .005 M solution of fluorescein in cyclohexanol was directionally solidified in a standard 10 x 10 x 45mm UV silica cuvette, using a bottom thermoelectric chilling device. Progress of the experiment was monitored by time lapse photography. During flight (SPAR I) the camera malfunctioned and only one quarter of the expected data were collected. Comparison of flight and ground specimens indicated that: (1) The dark green layer observed ahead of the solid-liquid interface which is most likely the solute-enriched zone, appears to be wider in the flight specimen; (2) Parasitic nucleation ahead of the solid-liquid interface in the flight sample led to an irregularly shaped interface, smaller grain size, equiaxed grain morphology and a larger average macroscopic growth rate; (3) The formation of equiaxed grains ahead of the solid-liquid interface in the flight specimen may be attributed to ordered islands within the liquid, which survived remelting because of the low degree of superheating (approximately equal to 1.5 C), did not settle because of reduced gravity and acted as nuclei during cooling.
New trace element analyses of 25 basalt samples from a vertical traverse in an 11 m thick flow of Icelandic tholeiite show compositional differences which exceed analytical uncertainties and are random with respect to height. These variations suggest a short-range segregation model in which the amounts of phenocrysts, groundmass materials, and residual liquid vary randomly in different samples of the flow; a least-squares method is applied to determine if these variations reflect different proportions of crystallizing phases and residual liquid. Monte Carlo computations indicate that short-range segregation results in inhomogeneity of a magnitude of interflow compositional differences; this causes incoherence in elements with different geochemical behaviors while preserving coherence in elements of similar behavior.
Comet nucleus sample return mission and other return missions from planets and satellites need equipment for handling and analysis of icy samples at low temperatures under vacuum or protective gas. Two methods are reported which were developed for analysis of small icy samples and which are modified for larger samples in cometary matter simulation experiments (KOSI). A conventional optical cryostat system was modified to allow for transport of samples at 5 K, ion beam irradiation, and measurement in an off-line optical spectrophotometer. The new system consists of a removable window plug containing nozzles for condensation of water and volatiles onto a cold finger. This plug can be removed in a vacuum system, changed against another plug (e.g., with other windows (IR, VIS, VUV) or other nozzles). While open, the samples can be treated under vacuum with cooling by manipulators (cut, removal, sample taking, irradiation with light, photons, or ions). After bringing the plug back, the samples can be moved to another site of analysis. For handling the 30 cm diameter mineral-ice samples from the KOSI experiments an 80x80x80 cm glove box made out of plexiglass was used. The samples were kept in a liquid nitrogen bath, which was filled from the outside. A stream a dry N2 and evaporating gas from the bath purified the glove box from impurity gases and, in particular, H2O, which otherwise would condense onto the samples.
The Cassini mission has revealed Titan to be one of the most Earthlike worlds in the Solar System complete with many of the same surface features including lakes, river channels, basins, and dunes. But unlike Earth, the materials and fluids on Titan are composed of cryogenic organic compounds with lakes of liquid methane and ethane. One of the potential mission concepts to explore Titan is to land a floating platform on one of the Titan Lakes and determine the local lake chemistry. In order to accomplish this within the expected mass volume and power budgets there is a need to pursue the development for a low power lightweight cryogenic valves which can be used along with vacuum lines to sample lake liquid and to distribute to various instruments aboard the Lander. To meet this need we have initiated the development of low power cryogenic valves and actuators based on a single crystal piezoelectric flextensional stacks produced by TRS Ceramics Inc. Since the origin of such high electromechanical properties of Relaxor-PT single crystals is due to the polarization rotation effect, (i.e., intrinsic contributions), the strain per volt decrease at cryogenic temperatures is much lower than in standard Lead Zirconate Titanate (PZT) ceramics. This makes them promising candidates for cryogenic actuators with regards to the stroke for a given voltage. This paper will present our Titan Lake Sampling and Sample Handling system design and the development of small cryogenic piezoelectric valves developed to meet the system specifications.
Thirty-two jet and diesel fuel samples of varying chemical composition and physical properties were prepared from oil shale and coal syncrudes. Hydrocarbon types in these samples were determined by a fluorescent indicator adsorption analysis, and the results from three laboratories are presented and compared. Two methods of rapid high performance liquid chromatography were used to analyze some of the samples, and these results are also presented and compared. Two samples of petroleum-based Jet A fuel are similarly analyzed.
Containerless processing is an important tool for thermophysical property measurements and materials research. The freedom from a crucible allows processing of liquid materials in a metastable undercooled state, as well as allowing processing of high temperature and highly reactive melts. Electrostatic levitation (ESL) is a containerless method which provides a number of unique advantages, including the decoupling of positioning force from sample heating, the ability to operate in ultra-high vacuum or at moderate gas pressure (approximately 3 atm), and the ability to process non-conducting materials. ESL also has the potential to reduce internal flow velocities below those possible with electromagnetic, acoustic, or aero-acoustic techniques. The ESL facility at NASA's Marshall Space Flight Center (MSFC) is in use for thermophysical property measurements and materials research by a number of different internal and external investigators. The methods for obtaining access to the facility, as well as a summary of current capabilities and some future directions will be discussed. In electrostatic levitation, the acceleration of gravity (or residual acceleration in reduced gravity) is opposed by the action of an applied electric field on a charged sample. This positioning method is applicable to any material which can be electrically charged, whether solid or liquid, conducting, or insulating. Because the position of the sample is unstable, a 3-dimensional active control loop rapidly adjusts the applied field to maintain levitation and minimize motion of the sample. Heating lasers melt the sample, and may be adjusted to maintain specified thermal profiles. Microgravity allows electrostatic levitation to work even more effectively. With the need to cancel less than 1 milli-g, the applied field required is reduced from approximately 10 MV/m to approximately 10 kV/m. Alternatively, a microgravity ESL can position larger samples than is possible on the ground, or it can position samples which maintain their charge poorly. Microgravity also reduces the effects of buoyant convection and sedimentation. In the MSFC ESL, many different classes of experiments and measurements have been demonstrated in collaboration with many investigators. These capabilities include heat capacity measurement, phase diagram determination, and nucleation and growth experiments including nucleation rate, TTT curves, and phase selection. We have demonstrated the capability of triggering recalescence of an undercooled liquid sample without loss of levitation. Currently under development are techniques for measuring the surface tension, viscosity, and density of levitated samples, as well as other thermophysical properties. Expanded levitation capabilities including various gas environments for sample processing, sample rotation control and management of thermal gradients are under development for the MSFC ESL. Containerless processing allows research on materials which may not be processed any other way. Electrostatic levitation extends the range of containerless processing to include many materials and classes of materials which cannot be processed by conventional electromagnetic, acoustic, or aerodynamic levitation techniques.
Future use of large size Kaufman thrusters and thruster arrays will impose new design requirements for porous plug type vaporizers. Larger flow rate coupled with smaller pores to prevent liquid intrusion will be desired. This paper presents the results of testing samples of porous tungsten for flow rate, liquid intrusion pressure level, and mechanical strength. Nitrogen gas was used in addition to mercury flow for approximate calibration. Liquid intrusion pressure levels will require that flight thruster systems with long feed lines have some way (a valve) to restrict dynamic line pressures during launch.
There are no existing ultra-sterile lab-on-a-chip systems that can accept solid samples and perform complete chemical analyses without human intervention. The proposed solution is to demonstrate completely automated lab-on-a-chip manipulation of powdered solid samples, followed by on-chip liquid extraction and chemical analysis. This technology utilizes a newly invented glass micro-device for solid manipulation, which mates with existing lab-on-a-chip instrumentation. Devices are fabricated in a Class 10 cleanroom at the JPL MicroDevices Lab, and are plasma-cleaned before and after assembly. Solid samples enter the device through a drilled hole in the top. Existing micro-pumping technology is used to transfer milligrams of powdered sample into an extraction chamber where it is mixed with liquids to extract organic material. Subsequent chemical analysis is performed using portable microchip capillary electrophoresis systems (CE). These instruments have been used for ultra-highly sensitive (parts-per-trillion, pptr) analysis of organic compounds including amines, amino acids, aldehydes, ketones, carboxylic acids, and thiols. Fully autonomous amino acid analyses in liquids were demonstrated; however, to date there have been no reports of completely automated analysis of solid samples on chip. This approach utilizes an existing portable instrument that houses optics, high-voltage power supplies, and solenoids for fully autonomous microfluidic sample processing and CE analysis with laser-induced fluorescence (LIF) detection. Furthermore, the entire system can be sterilized and placed in a cleanroom environment for analyzing samples returned from extraterrestrial targets, if desired. This is an entirely new capability never demonstrated before. The ability to manipulate solid samples, coupled with lab-on-a-chip analysis technology, will enable ultraclean and ultrasensitive end-to-end analysis of samples that is orders of magnitude more sensitive than the ppb goal given in the Science Instruments.
We performed a series of experiments on 0.518 millimeter PMMA spheres suspended in an index matching mixture of decalin and tetralin the microgravity environment provided by the Shuttle Columbia on mission STS-73. The samples ranged in concentration from 0.49 to 0.62. volume fraction (phi) of spheres, which covers the range in which liquid, coexistence, solid and glass phases are expected from Earth bound experiments. Light scattering was used to probe the static structure, and the particle dynamics. Digital and 35 mm photos provided information on the morphology of the crystals. In general, the crystallites grew considerably larger (roughly an order of magnitude larger) than the same samples with identical treatment in 1 g. The dynamic light scattering shows the typical short time diffusion and long time caging effects found in 1 g. The surprises that were encountered in microgravity include the preponderance of random hexagonal close packed (RHCP) structures and the complete absence of the expected face centered cubic (FCC) structure, existence of large dendritic crystals floating in the coexistence samples (where liquid and solid phases coexist) and the rapid crystallization of samples which exist only in glass phase under the influence of one g. These results suggest that colloidal crystal growth is profoundly effected by gravity in yet unrecognized ways. We suspect that the RCHP structure is related to the nonequilibrium growth that is evident from the presence of dendrites. An analysis of the dendritic growth instabilities is presented within the framework of the Ackerson-Schatzel equation.
This paper presents experimental results for the liquid hydrogen bubble point tests using warm pressurant gases conducted at the Cryogenic Components Cell 7 facility at the NASA Glenn Research Center in Cleveland, Ohio. 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. Three fine mesh screen samples (325 x 2300, 450 x 2750, 510 x 3600) were tested in liquid hydrogen using cold and warm noncondensible (gaseous helium) and condensable (gaseous hydrogen) pressurization schemes. Gases were conditioned from 0 to 90 K above the liquid temperature. Results clearly indicate a degradation in bubble point pressure using warm gas, with a greater reduction in performance using condensable over noncondensible 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.