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The primary focus of this study was organic contamination introduced into those Mars samples that would be delivered to sensitive analytical instruments after processing by lander acquisition and sampling devices.
Ten years in the making the Center for Isotope Cosmochemistry and Geochronology (CICG) at NASA Johnson Space Center is designed to be a cooperative analytical facility where novel techniques are developed and performed. Our team works collaboratively to operate this integrated lab suite comprising sample preparation, metal-free clean chemistry, and mass spectrometers to measure a wide variety of elements and isotopes in astromaterials. Contamination control is enacted throughout by a positive pressure cascade of HEPA filtered air, weekly surface cleaning and particle counting. Astromaterials processing is performed with application-specific mortar and pestles, heavy liquid separation, a Frantz magnetic separator, as well as hand-picking using optical microscopes in laminar flow boxes. Microsampling is also carried out using a New Wave MicroMill. Elements for isotopic analysis are isolated from acid-digested samples using ion-exchange chromatography. Cross-contamination is minimized with dedicated laminar flow boxes and labware for different purification protocols. Instrumentation includes a ThermoFisher Element XR inductively coupled plasma mass spectrometer (ICP-MS) for quantification of elemental concentrations in dissolved sample solutions. For in situ analysis, a Teledyne Photon Machines Analyte Excite+ laser ablation system is coupled to the Element XR. The ThermoFisher Triton thermal ionization mass spectrometer (TIMS) is used to measure the isotopic composition of elements such as CA, K, Cr, Rb, Sr, Sm, Nd at high precision in processed samples. For a more diverse range of isotopic analyses, CICG houses a Nu Sapphire 1700 multi-collector inductively coupled plasma mass spectrometer (MC-ICP-MS), which is a large geometry instrument with a multi-pole collision cell for interference removal. An Applied Spectra Instruments J200 femto-second laser is planned for install this Fall and will be coupled to the Nu Sapphire 1700. NASA’s Internal Scientist Funding Model (ISFM)supports this facility. Advanced analytical geochemistry techniques are applied to targeted astromaterials to address important problems in planetary sciences, with a longer-term goal of preparing for samples collected and returned by space missions. CICG is open to collaborations on projects that utilize the facility’s unique capabilities and are within its research scope. We are particularly eager to support and share expertise with the next generation of planetary scientists.
The Mars Science Laboratory (MSL) Curiosity Rover carries a suite of instruments, one of which is the Sample Analysis at Mars (SAM) experiment. SAM is devoted to the in situ molecular analysis of gases evolving from solid samples collected by Curiosity on Mars surface/sub-surface. Among its three analytical devices, SAM has a gaschromatograph coupled to a quadrupole mass spectrometer (GC-QMS). The GC-QMS is devoted to the separation and identification of organic and inorganic material. Before proceeding to the GC-QMS analysis, the solid sample collected by Curiosity is subjected to a thermal treatment thanks to the pyrolysis oven to release the volatiles into the gas processing system. Depending on the sample, a derivatization method by wet chemistry: MTBSTFA of TMAH can also be applied to analyze the most refractory compounds. The GC is able to separate the organic molecules which are then detected and identified by the QMS (Figure 1). For the second time after the Viking landers in 1976, SAM detected chlorinated organic compounds with the pyrolysis GC-QMS experiment. The detection of perchlorates salts (ClO4-) in soil at the Phoenix Landing site suggests that the chlorohydrocarbons detected could come from the reaction of organics with oxychlorines. Indeed, laboratory pyrolysis experiments have demonstrated that oxychlorines decomposed into molecular oxygen and volatile chlorine (HCl and/or Cl2) when heated which then react with the organic matter in the solid samples by oxidation and/or chlorination processes.
A sampling strategy and a signal processing technique are proposed to overcome Non Uniform Beam Filling (NUBF) errors on mean Doppler velocity measurements made by spaceborne weather radars.
A method for producing a uniform, highly textured surface on oxygen-free, high conductivity (OFHC) copper by ion bombardment using sputtered molybdenum as a texture-inducing masking film was developed and used to provide samples for study. The purpose was to develop a basically OFHC copper surface having very low secondary electron emission characteristics. Surfaces having low secondary electron emission are a requirement for the electrodes of very high efficiency multistage depressed collectors (MDC's). Such MDC's are used in microwave amplifier traveling wave tubes for space communications and other applications. OFHC copper is the material most commonly used for MDC electrodes because it has high thermal conductivity, it is easy to machine, and its fabrication and brazing procedures are well established. However, its untreated surface displays relatively very high levels of secondary electron emissions. Textured OFHC copper samples were tested for true secondary electron emission and relative reflected primary electron yield at primary electron beam energy levels from 200 to 2000 eV and at direct (0 deg) to oblique (60 deg) beam impingement angles. The test results for three of the samples, each of which was processed in a slightly different way, are compared with each other and with test results for a machined OFHC copper sample. Although the textured samples are not represented here as having been processed optimally, their measured secondary electron emission characteristics are significantly lower than those of the untreated OFHC copper sample over the range of conditions studied. Importantly, the relative reflected primary electron yield of one of the textured samples is conspicuously lower than that of the others. Clearly, with further development, the molybdenum-masked ion-textured OFHC copper surface will be a promising material for high-efficiency MDC electrodes.
A container designed for storing samples of hazardous material features a double wall, part of which is sacrificed during an explosion-welding process in which the container is sealed and transferred to a clean environment. The major advantage of this container sealing process is that once the samples have been sealed inside, the outer wall of what remains of the container is a clean surface that has not come into contact with the environment from which the samples were taken. Thus, there is no need to devise a decontamination process capable of mitigating all hazards that might be posed by unanticipated radioactive, chemical, and/or biological contamination of the outside of the container. The container sealing method was originally intended to be used to return samples from Mars to Earth, but it could also be used to store samples of hazardous materials, without the need to decontaminate its outer surface. The process stages are shown. In its initial double-wall form, the volume between the walls is isolated from the environment; in other words, the outer wall (which is later sacrificed) initially serves to protect the inner container from contamination. The sample is placed inside the container through an opening at one end, then the container is placed into a transfer dock/lid. The surfaces that will be welded together under the explosive have been coated with a soft metallic sacrificial layer. During the explosion, the sacrificial layer is ejected, and the container walls are welded together, creating a strong metallic seal. The inner container is released during the same event and enters the clean environment.
The basic concept of aliasing is this: Converting analog data into digital data requires sampling the signal at a specific rate, known as the sampling frequency. The result of this conversion process is a new function, which is a sequence of digital samples. This new function has a frequency spectrum, which contains all the frequency components of the original signal. The Fourier transform mathematics of this process show that the frequency spectrum of the sequence of digital samples consists of the original signal s frequency spectrum plus the spectrum shifted by all the harmonics of the sampling frequency. If the original analog signal is sampled in the conversion process at a minimum of twice the highest frequency component contained in the analog signal, and if the reconstruction process is limited to the highest frequency of the original signal, then the reconstructed signal accurately duplicates the original analog signal. It is this process that can give birth to aliasing.
One very important tool in the analysis of biogenic, and potentially biogenic, samples is the study of their stable isotope distributions. The isotope distribution of a sample depends on the process(es) that created it. One important application of the analysis of C & N stable isotope ratios has been in the determination of whether organic matter in a sample is of biological origin or was produced abiotically. For example, the delta C-13 of organic material found embedded in phosphate grains was cited as a critical part of the evidence for life in 3.8 billion year old samples. The importance of such analysis in establishing biogenicity was highlighted again by the role this issue played in the recent debate over the validity of what had been accepted as the Earth s earliest microfossils. These kinds of analysis imply a comparison with the fractionation that one would have seen if the organic material had been produced by alternative, abiotic, pathways. Could abiotic reactions account for the same level of fractionation? Additionally, since the fractionation can vary between different abiotic reactions, understanding their fractionations can be important in distinguishing what reactions may have been significant in the formation of different abiological samples (such as extraterrestrial samples). There is however, a scarcity of data on the fractionation of carbon and nitrogen by abiotic reactions. In order to interpret properly what the stable isotope ratios of samples tell us about their biotic or abiotic nature, more needs to be known about how abiotic reactions fractionate C and N. Carbon isotope fractionations have been studied for a few abiotic processes. These studies presumed the presence of a reducing atmosphere, focusing on reactions involving spark discharge, W photolysis of reducing gas mixtures, and cyanide polymerization in the presence of ammonia. They did find that the initial products showed a depletion in I3C with values in the range of a few per mil to as low as -60 % (potentially comparable to that which accompanies the biosynthesis of organic matter). We need to understand what kind of fractionations are observed with reactions under the non-reducing or mildly reducing conditions now thought to be present on the early Earth. While nitrogen is receiving increased attention as a tool for these kinds of analyses, almost nothing is known about the isotope fractionation that one would expect for abiotic sources of fixed/reduced nitrogen. This project will measure the fixation from a series of abiotic reactions that may have been present on the early Earth (and other terrestrial planets) and produced organic material that could have ended up in the rock record. The work will look at a number of reactions, under a non- reducing, or mildly reducing, atmosphere, covering sources of prebiotic organic C & N from shock heating, to photochemistry, to hydrothermal reactions. Some reactions that we plan to study are; Shock heating of a non-reducing atmosphere to produce CO and NO (in collaboration with Chris McKay), formation of formaldehyde (and related compounds) from COY the formation of ammonia from nitrogen oxides (ultimately from NO) by ferrous iron reduction, and the hydrothermal synthesis of compounds including the hydrocarboxylation/hydrocarbonylation reaction (in collaboration with George Cody), reactions of oxalate to form hydrocarbons and other oxygenated compounds and the formation of lipids from oxalic/formic acid (in collaboration with Tom McCollom), and reactions of carbon monoxide & carbon dioxide with N2, ammonia or nitritehitrate to form hydrogen cyanide, nitriles, ammonia/amines and nitrous
Autocorrelation based spectral moment estimators are typically derived using the Fourier transform relationship between the power spectrum and the autocorrelation function along with using either an assumed form of the autocorrelation function, e.g., Gaussian, or a generic complex form and applying properties of the characteristic function. Passarelli has used a series expansion of the general complex autocorrelation function and has expressed the coefficients in terms of central moments of the power spectrum. A truncation of this series will produce a closed system of equations which can be solved for the central moments of interest. The autocorrelation function at various lags is estimated from samples of the random process under observation. These estimates themselves are random variables and exhibit a bias and variance that is a function of the number of samples used in the estimates and the operational signal-to-noise ratio. This contributes to a degradation in performance of the moment estimators. This dissertation investigates the use autocorrelation function estimates at higher order lags to reduce the bias and standard deviation in spectral moment estimates. In particular, Passarelli's series expansion is cast in terms of an overdetermined system to form a framework under which the application of additional autocorrelation function estimates at higher order lags can be defined and assessed. The solution of the overdetermined system is the least squares solution. Furthermore, an overdetermined system can be solved for any moment or moments of interest and is not tied to a particular form of the power spectrum or corresponding autocorrelation function. As an application of this approach, autocorrelation based variance estimators are defined by a truncation of Passarelli's series expansion and applied to simulated Doppler weather radar returns which are characterized by a Gaussian shaped power spectrum. The performance of the variance estimators determined from a closed system is shown to improve through the application of additional autocorrelation lags in an overdetermined system. This improvement is greater in the narrowband spectrum region where the information is spread over more lags of the autocorrelation function. The number of lags needed in the overdetermined system is a function of the spectral width, the number of terms in the series expansion, the number of samples used in estimating the autocorrelation function, and the signal-to-noise ratio. The overdetermined system provides a robustness to the chosen variance estimator by expanding the region of spectral widths and signal-to-noise ratios over which the estimator can perform as compared to the closed system.
Japan Aerospace Exploration Agency (JAXA) will launch a spacecraft in 2024 for a sample return mission from Phobos (Martian Moons eXploration: MMX). The major scientific goals of MMX are to constrain (1) the origin of Phobos and Deimos and (2) the evolution of the Mars-moon system [1]. The touchdown operations are planned to be performed twice at different landing sites on the Phobos surface to collect > 10 g of the surface materials [2]. After the return to the Earth, the Phobos samples will be collected from the individual sample canisters and introduced to the clean chamber installed at ISAS (Institute of Space and Astronautical Science). The Sample Analysis Working Team (SAWT) of MMX designed the procedure of Phobos sample analysis mainly conducted by the initial analysis teams [3]. For the next step, the SAWT will define the procedure of the curation process (mostly non-destructive analysis) of the Phobos samples, which will be presented here. The protocols of the Phobos sample curation is illustrated in figure 1. First, the headspace gas from the sample container will be collected during the Quick Analysis phase. The Quick Analysis will be operated by the sampler and curation teams in ISAS/JAXA. The terrestrial leak and contamination from the sampling systems will be tested using a quadrupole mass spectrometer equipped with a gas sampling system. Second, the bulk Phobos sample will be observed in the clean chamber under purified-N2 gas with an ambient condition (Pre-basic Characterization). This phase will be operated by the curation team in ISAS/JAXA and the instrument team of the MMX mission. The consistency between the data from the instruments in the clean chamber and the spacecraft will then be evaluated. Subsequently, the curation will distribute the small amount of Phobos samples to the Initial analysis team of MMX to conduct the "Preliminary Examination". The objectives of the preliminary examination are to provide (1) feedback on the subsequent sample allocation process, (2) preliminary scientific results that will address parts of MMX mission goals, and (3) evaluation of the sampling system and terrestrial alteration on Phobos samples. Because multiple models are proposed for the origin of Phobos [1] (e.g., giant impact, the capture of asteroids), the chemical and mineralogical characteristics of Phobos must be assessed before the allocation of the samples to the individual initial analysis teams. Simultaneously, the curation team in JAXA will observe the individual grains and aliquots of the samples in the clean chamber (Basic Characterization).
The Catalog of Apollo 17 Rocks is a set of volumes that characterize each of 334 individually numbered rock samples (79 larger than 100 g) in the Apollo 17 collection, showing what each sample is and what is known about it. Unconsolidated regolith samples are not included. The catalog is intended to be used by both researchers requiring sample allocations and a broad audience interested in Apollo 17 rocks. The volumes are arranged geographically, with separate volumes for the South Massif and Light Mantle, the North Massif, and two volumes for the mare plains. Within each volume, the samples are arranged in numerical order, closely corresponding with the sample collection stations. The present volume, for the South Massif and Light Mantle, describes the 55 individual rock fragments collected at Stations two, two-A, three, and LRV-five. Some were chipped from boulders, others collected as individual rocks, some by raking, and a few by picking from the soil in the processing laboratory. Information on sample collection, petrography, chemistry, stable and radiogenic isotopes, rock surface characteristics, physical properties, and curatorial processing is summarized and referenced as far as it is known up to early 1992. The intention has been to be comprehensive: to include all published studies of any kind that provide information on the sample, as well as some unpublished information. References which are primarily bulk interpretations of existing data or mere lists of samples are not generally included. Foreign language journals were not scrutinized, but little data appears to have been published only in such journals. We have attempted to be consistent in format across all of the volumes, and have used a common reference list that appears in all volumes. Where possible, ages based on Sr and Ar isotopes have been recalculated using the 'new' decay constants recommended by Steiger and Jager; however, in many of the reproduced diagrams the ages correspond with the 'old' decay constants. In this volume, mg' or Mg' = atomic Mg/(Mg +Fe).
The effect of power/temperature step stress when applied to the transistor JANTX2N2905A manufactured by Texas Instruments and Motorola is reported. A total of 48 samples from each manufacturer was submitted to the process outlined. In addition, two control sample units were maintained for verification of the electrical parametric testing. All test samples were subjected to the electrical tests outlined in Table 2 after completing the prior power/temperature step stress point.
Power/temperature step stress was applied to the transistor JANTX2N2432A manufactured by Crystalonics and Texas Instruments. A total of 48 samples from each manufacturer were submitted to the process outlined. In addition, two control sample units were maintained for verification of the electrical parametric testing. All test samples were subjected to the electrical tests after completing the prior power/temperature step stress point.
The effect of power/temperature step stress when applied to the switching diode JANTX1N5554 manufactured by Semtech and Micro Semiconductor was evaluated. A total of 48 samples from each manufacturer were submitted to the process outlined. In addition, two control sample units were maintained for verification of the electrical parametric testing.
Power/temperature step stress was applied to the dual transistor JANTX2N2219A manufactured by Texas Instruments and National Semiconductor. A total of 48 samples from each manufacturer were submitted to the process outlined. In addition, two control sample units were maintained for verification of the electrical parametric testing. All test samples were subjected to electrical tests after completing the prior power/temperature step stress point.
Data compiled for the purpose of evaluating the effect of power/temperature step stress when applied to the diode JANTX1N5420 manufactured by Unitrode and Micro-Semiconductor is presented. A total of 48 samples from each manufacturer was submitted to the processes outlined. In addition, two control sample units were maintained for verification of the electrical parametric testing.
This paper presents a statistical test for detecting significant differences between two random count accumulations. The null hypothesis is that the two samples share a common random arrival process with a mean count proportional to each sample's exposure. The model represents the partition of N total events into two counts, A and B, as a sequence of N independent Bernoulli trials whose partition fraction, f, is determined by the ratio of the exposures of A and B. The detection of a significant difference is claimed when the background (null) hypothesis is rejected, which occurs when the observed sample falls in a critical region of (A, B) space. The critical region depends on f and the desired significance level, alpha. The model correctly takes into account the fluctuations in both the signals and the background data, including the important case of small numbers of counts in the signal, the background, or both. The significance can be exactly determined from the cumulative binomial distribution, which in turn can be inverted to determine the critical A(B) or B(A) contour. This paper gives efficient implementations of these tests, based on lookup tables. Applications include the detection of clustering of astronomical objects, the detection of faint emission or absorption lines in photon-limited spectroscopy, the detection of faint emitters or absorbers in photon-limited imaging, and dosimetry.
Research is being done at the Glenn Research Center (GRC) developing new kinds of batteries that do not depend on a solution. Currently, batteries use liquid electrolytes containing lithium. Problems with the liquid electrolyte are (1) solvents used can leak out of the battery, so larger, more restrictive, packages have to be made, inhibiting the diversity of application and decreasing the power density; (2) the liquid is incompatible with the lithium metal anode, so alternative, less efficient, anodes are required. The Materials Department at GRC has been working to synthesize polymer electrolytes that can replace the liquid electrolytes. The advantages are that polymer electrolytes do not have the potential to leak so they can be used for a variety of tasks, small or large, including in the space rover or in space suits. The polymers generated by Dr. Mary Ann Meador's group are in the form of rod -coil structures. The rod aspect gives the polymer structural integrity, while the coil makes it flexible. Lithium ions are used in these polymers because of their high mobility. The coils have repeating units of oxygen which stabilize the positive lithium by donating electron density. This aids in the movement of the lithium within the polymer, which contributes to higher conductivity. In addition to conductivity testing, these polymers are characterized using DSC, TGA, FTIR, and solid state NMR. Solid state NMR is used in classifying materials that are not soluble in solvents, such as polymers. The NMR spins the sample at a magic angle (54.7') allowing the significant peaks to emerge. Although solid state NMR is a helpful technique in determining bonding, the process of preparing the sample and tuning it properly are intricate jobs that require patience; especially since each run takes about six hours. The NMR allows for the advancement of polymer synthesis by showing if the expected results were achieved. Using the NMR, in addition to looking at polymers, allows for participation on a variety of other projects, including aero-gels and carbon graphite mat en als. The goals of the polymer electrolyte research are to improve the physical properties of the polymers. This includes improving conductivity, durability, and expanding the temperature range over which it is effective. Currently, good conductivity is only present at high temperatures. My goals are to experiment with different arrangements of rods and coils to achieve these desirable properties. Some of my experiments include changing the number of repeat units in the polymer, the size of the diamines, and the types of coil. Analysis of these new polymers indicates improvement in some properties, such as lower glass transition temperature; however, they are not as flexible as desired. With further research we hope to produce polymers that encompass all of these properties to a high degree.