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At least 91 records · Page 5
All sourcesNASA NTRSDOE OSTI
NASA NTRS1972

Tetraperchlorate of methane

The preparation of the tetraperchlorate of methane (TPM) was attempted. Displacement of halogen from carbon tetrahalides was accomplished with either CCl4 or CBr4 using the halogen perchlorates, ClOClO3, and BOClO3. Although the displacement process was successful, the generated carbon perchlorate intermediates were not isolated. Instead, these species decomposed to COCl2, CO2, and Cl2O7. The vigorous displacement reaction that often occurred required moderation. Fluorocarbon solvents and chlorine perchlorate were successfully tested for compatibility, permitting their use in these synthetic reactions. While the sought for moderating effect was obtained, the net result of the displacement of halogen from CX sub 4 substrates was the same as before. Thus only CO2, COCl2, and Cl2O7 were isolated.

Schack, C. J.↗
NASA NTRS2002

Pure Water From a Pure Genius

Ammonium perchlorate is widely used throughout the aerospace, munitions, and pyrotechnics industries as a primary ingredient in solid rocket and missile propellants, fireworks, and explosive charges. This highly soluble salt has tainted soils and water sources all over the world, and is believed to be an endocrine disrupter, adversely affecting the growth patterns of a fetus or a young child. UMPQUA Research Company (URC), once a small drinking water testing laboratory and a research and development contractor for NASA's manned spaceflight applications, has evolved to become a leader in water purification and analysis. With a total of 11 patents issued for new technologies created by URC under NASA SBIR contracts and a 25-year commitment to water recycling, the company clearly possessed the qualifications necessary to tackle the presence of perchlorate in water. An SBIR contract with NASA's Marshall Space Flight Center that concentrated on the stringent water quality requirements of long-term, manned spaceflight was the source for URC's process and catalyst to facilitate the destruction of perchlorate and nitrate in water. URC licensed the rights of its unique reduction reaction process to Calgon Carbon Corporation for use with the company's perchlorate/nitrate remediation process, otherwise known as ISEP(R).

Source record↗
NASA NTRS2013

Investigating the Origin of Chlorohydrocarbons Detected by the Sample Analysis at Mars (SAM) Instrument at Rocknest

The search for organic compounds on Mars, including molecules of either abiotic or biological origin is one of the key goals of the Mars Science Laboratory (MSL) mission. Previously the Viking and Phoenix Lander missions searched for organic compounds, but did not find any definitive evidence of martian organic material in the soils. The Viking pyrolysis gas chromatography mass spectrometry (GCMS) instruments did not detect any organic compounds of martian or exogenous origin above a level of a few parts-per-billion (ppb) in the near surface regolith at either landing site [1]. Viking did detect chloromethane and dichloromethane at pmol levels (up to 40 ppb) after heating the soil samples up to 500 C (Table 1), although it was originally argued that the chlorohydrocarbons were derived from cleaning solvents used on the instrument hardware, and not from the soil samples themselves [1]. More recently, it was suggested that the chlorohydrocarbons detected by Viking may have been formed by oxidation of indigenous organic matter during pyrolysis of the soil in the presence of perchlorates [2]. Although it is unknown if the Viking soils contained perchlorates, Phoenix did reveal relatively high concentrations (~0.6 wt%) of perchlorate salt in the icy regolith [3], therefore, it is possible that the chlorohydrocarbons detected by Viking were produced, at least partially, during the experiments [2,4]. The Sample Analysis at Mars (SAM) instrument suite on MSL analyzed the organic composition of the soil at Rocknest in Gale Crater using a combination of pyrolysis evolved gas analysis (EGA) and GCMS. One empty cup procedural blank followed by multiple EGA-GCMS analyses of the Rocknest soil were carried out. Here we will discuss the results from these SAM measurements at Rocknest and the steps taken to determine the source of the chlorohydrocarbons.

Glavin, D.↗
NASA NTRS2015

The Icebreaker Mission to Search for Life on Mars

The search for evidence of life on Mars is the ultimate motivation for its scientific exploration. The results from the Phoenix mission indicate that the high N. latitude ice-rich regolith at low elevations is likely to be a recently habitable place on Mars [Stoker et al., 2010]. The near-surface ice likely provided adequate water activity during periods of high obliquity, 3 to 10 Myr ago. Carbon dioxide and nitrogen are present in the atmosphere, and nitrates may be present in the soil. Together with iron in basaltic rocks and perchlorate in the soil they provide carbon and energy sources, and oxidative power to drive metabolism. Furthermore, the presence of organics is possible, as thermally reactive perchlorate would have prevented their detection by Viking and Phoenix. The Mars Icebreaker Life mission [McKay et al., 2013] focuses on the following science goals: (1) Search for biomolecular evidence of life; (2) Search for organic matter from either exogeneous or endogeneous sources using methods that are not effected by the presence of perchlorate; (3) Characterize oxidative species that produced reactivity of soils seen by Viking; and 4) Assess the habitability of the ice bearing soils. The Icebreaker Life payload (Figure 1) includes a 1-m rotary percussive drill that brings cuttings samples to the surface where they are delivered to three instruments (Fig. 1), the Signs of Life Detector (SOLID) [Parro et al., 2011] for biomolecular analysis, Laser Desorption Mass Spectrometer (LDMS) [??? 2015]) for broad spectrum organic analysis, and Wet Chemistry Laboratory (WCL) [Hecht et al., 2009] for detecting soluble species of nutrients and reactive oxidants. The Icebreaker payload fits on the Phoenix spacecraft and can land at the well-characterized Phoe-nix landing site in 2020 in a Discovery-class mission.

Carbon dioxide and nitrogen↗
NASA NTRS2017

Oxychlorine Species in Gale Crater and Broader Implications for Mars

Of 15 samples analyzed to date, the Sample Analysis at Mars (SAM) instrument on the Mars Science Laboratory (MSL) has detected oxychlorine compounds (perchlorate or chlorate) in 12 samples. The presence of oxychlorine species is inferred from the release of oxygen at temperatures less than 600degC and HCl between 350-850degC when a sample is heated to 850degC. The O2 release temperature varies with sample, likely caused by different cations, grain size differences, or catalytic effects of other minerals. In the oxychlorine-containing samples, perchlorate abundances range from 0.06 +/- 0.03 to 1.15 +/- 0.5 wt% Cl2O7 equivalent. Comparing these results to the elemental Cl concentration measured by the Alpha Particle X-ray Spectrometer (APXS) instrument, oxychlorine species account for 5-40% of the total Cl present. The variation in oxychlorine abundance has implications for their production and preservation over time. For example, the John Klein (JK) and Cumberland (CB) samples were acquired within a few meters of each other and CB contained approximately1.2 wt% Cl2O7 equivalent while JK had approximately 0.1 wt%. One difference between the two samples is that JK has a large number of veins visible in the drill hole wall, indicating more post-deposition alteration and removal. Finally, despite Cl concentrations similar to previous samples, the last three Murray formation samples (Oudam, Marimba, and Quela) had no detectable oxygen released during pyrolysis. This could be a result of oxygen reacting with other species in the sample during pyrolysis. Lab work has shown this is likely to have occurred in SAM but it is unlikely to have consumed all the O2 released. Another explanation is that the Cl is present as chlorides, which is consistent with data from the ChemCam (Chemical Camera) and CheMin (Chemistry and Mineralogy) instruments on MSL. For example, the Quela sample has approximately1 wt% elemental Cl detected by APXS, had no detectable O2 released, and halite (NaCl) has been tentatively identified in CheMin X-ray diffraction data. These data show that oxychlorines are likely globally distributed on Mars but the distribution is heterogenous depending on the perchlorate formation mechanism (production rate), burial, and subsequent diagenesis

Ming, Douglas W.↗
NASA NTRS2020

Evidence for Adsorption of Chlorine Species on Iron (III)(Hydr)oxides in the Sheepbed Mudstone, Gale Crater, Mars

Ancient aquatic environments in Yellowknife Bay, Gale crater, Mars, could create favorable conditions for adsorption of chlorine compounds (perchlorate and chloride) on Fe (III) (hydr)oxides present in the Sheepbed mudstone, such as akaganeite and ferrihydrite. In this work, 5.2 mM ClO4− and 1.7 to 12 mM Cl− were adsorbed onto ferrihydrite and 5.2 mM ClO4− was adsorbed onto akaganeite at ultraacidic (pH 2–2.5), acidic (pH 3.8–4.5), and near‐neutral (pH 6.2–7.7) pH. Samples were characterized by evolved gas analysis and compared to the data collected for the Cumberland sample from the Sheepbed mudstone. Evolved gas analysis showed that ferrihydrite with 0.5–1 wt.% ClO4− adsorbed under ultraacidic and acidic conditions had a well‐resolved O2 peak at 306 °C due to the thermal decomposition of adsorbed ClO4−. All akaganeite samples with 0.5 wt.% adsorbed ClO4− had a weak peak at 312 °C tentatively assigned to decomposing perchlorate. Evolved gas analysis demonstrated that 0.5–2 wt.% Cl− adsorbed on ferrihydrite at ultraacidic and acidic pH was the main contributor to HCl evolved at >470 °C. Comparison with martian observations indicated that the temperature of the O2 peak originating from ClO4− adsorbed on ferrihydrite matched well with the thermal evolution of O2 from the Cumberland. Evolved HCl originating from Cl− adsorbed on ferrihydrite was within the temperature range of the high‐temperature HCl release from Cumberland (~770 °C). These observations suggest that ferrihydrite containing adsorbed ClO4− and Cl− could exist in the mudstone. Experimental results are consistent with adsorption at acidic pH < 4 environments through postdepositional water‐rock interactions of ferrihydrite with acid‐sulfate groundwater containing dissolved chloride and perchlorate.

T. S. Peretyazhko↗
NASA NTRSDate not supplied

LIRA: Probing the Lunar Surface for Resources.

The thermal, compositional and electrical properties of the lunar regolith, such as the triboelectric properties of lunar dust, the volatile content and the thermophysical properties of the polar regolith are essential to understand from a scientific perspective as well as for resource extraction and hazard mitigation. Understanding these properties specifically requires in situ measurement, as these properties are inherent in the ambient environment. With the Lunar In situ Regolith Analyzer (LIRA) we will combine mature surface sensor technologies from previous spacecraft missions (TECP) with new sensors (ClO4- ) and battery capability to achieve a compact in situ analysis package. The surface instrument suite is adapted for lunar conditions from a sensor developed as part of the Microscopy, Electrochemistry, and Conductivity Analyzer (MECA) instrument on the 2007 Mars Phoenix mission, as well as supplemental sensors. • The Thermal and Electrical Conductivity Probe (TECP), flown on MECA/Phoenix, which measures heat capacity, thermal conductivity, electrical resistance, and electrical permittivity between needles inserted into the soil. The TECP also measured atmospheric humidity, a capability that will be retained to search for subsurface H2O ice. The Mars TECP weighed 100-gram and by definition was at TRL 9. The lunar version (LIRA) is TRL 4. • The Perchlorate (ClO4) sensor is based on the fluorescence property of perchlorate (Mg, Fe, Na). We added a light source to excite the perchlorate (ClO4) and a photo diode to collect the emission wavelength. A sun-shade over the photo diode blocks out the ambient light during day light hours. The unifying goal of LIRA is to deliver a complete, integrated experiment suite that investigates properties that must be measured in situ, and provides the capability to power the suite at night or in PSRs, as well as a means to simulate aspects of the diurnal transition by delivering an optical pulse to the surface with intensity comparable to sunlight. We describe the scientific context of LIRA, touching on the electrical state of the near-surface environment, the thermal properties of the undisturbed regolith, and the distribution, geochemistry, and mobility of water. We also address the exploration implications of the work, examining hazards and resources in the context of strategic knowledge gaps (SKGs).

Heather Smith↗
NASA NTRS2022

Rapid Radiolytic Degradation of Amino Acids in the Martian Shallow Subsurface: Implications for the Search for Extinct Life

Amino acids are fundamental to life as we know them as the monomers of proteins and enzymes. They are also readily synthesized under a variety of plausible prebiotic conditions and are common in carbon-rich meteorites. Thus, they represent a reasonable class of organics to target in the search for prebiotic chemistry or chemical evidence of life on Mars. However, regardless of their origin, amino acids and other organic molecules present in near-surface regolith and rocks on Mars can be degraded by exposure to cosmic rays that can penetrate to a depth of a few meters. We exposed several pure amino acids in dry and hydrated silicate mixtures and in mixtures of silicates with perchlorate salts to gamma radiation at various temperatures and radiation doses representative of the martian near-subsurface. We found that irradiation of amino acids mixed with dry silica powder increased the rate of amino acid radiolysis, with the radiolysis constants of amino acids in silicate mixtures at least a factor of 10 larger compared with the radiolysis constants of amino acids alone. The addition of perchlorate salts to the silicate samples or hydration of silicate samples further accelerated the rate of amino acid destruction during irradiation and increased the radiolysis constants by a factor of *1.5. Our results suggest that even low-molecular-weight amino acids could degrade in just *20 million years in the top 10 cm of the martian surface regolith and rock, and even faster if the material contains elevated abundances of hydrated silicate minerals or perchlorates. We did not detect evidence of amino acid racemization after gamma radiation exposure of the samples, which indicates that the chirality of some surviving amino acids may still be preserved. Our experimental results suggest serious challenges for the search of ancient amino acids and other potential organic biosignatures in the top 2 m of the martian surface.

Alexander A. Pavlov↗
NASA NTRS1968

Analytical and experimental studies of the steady state combustion mechanism of solid propellants

Our present state of understanding of the steady-state combustion mechanisms of solid propellants is reviewed. Attention is focused principally on heterogeneous propellants. Both experimental and theoretical work is discussed. The recent advances considered include studies of linear pyrolysis of propellant constituents, deflagration of exothermic oxidizers, combustion of oxidizer spheres in gaseous fuels, porous-bed combustion, reactions between gaseous fuel and gaseous oxidizer components, metal combustion, propellant strand burning, rocket motor combustion and microcinematographic experimentation. A theoretical analysis of a model of homogeneous propellant combustion is outlined in detail, with special emphasis placed on surface gasification laws and on flammability limits in nonadiabatic systems. Low pressure, moderate pressure, plateau and high pressure domains of combustion are identified for ammonium perchlorate composite propellants. It is concluded that a better foundation for investigating composite propellant combustion properties is available for ammonium perchlorate than for any other oxidizer. Avenues for potentially fruitful future research are recommended.

M Barrère↗
NASA NTRS1973

A new look at AP/composite propellant combustion

Some theoretical studies on the time-independent and oscillatory combustion of nonmetallized ammonium perchlorate (AP)/composite propellants are presented. A coherent and unified interpretation was made of the voluminous data available from experiments related to propellant combustion. Three fundamental hypotheses are introduced: the extent of propellant degradation at the vaporization step has to be specified through a scientific criterion; the condensed-phase degradation reaction of ammonium perchlorate to a vaporizable state is the overall rate-limiting step; gas-phase combustion rate is controlled by the mixing rate of fuel and oxidizer vapors. In the treatment of oscillatory combustion, the assumption of quasi-steady fluctuations in the gas phase is used to supplement these hypotheses.

Kumar, R. N.↗
NASA NTRS1974

Preparing oxidizer coated metal fuel particles

A solid propellant composition of improved efficiency is described which includes an oxidizer containing ammonium perchlorate, and a powered metal fuel, preferably aluminum or beryllium, in the form of a composite. The metal fuel is contained in the crystalline lattice framework of the oxidizer, as well as within the oxidizer particles, and is disposed in the interstices between the oxidizer particles of the composition. The propellant composition is produced by a process comprising the crystallization of ammonium perchlorate in water, in the presence of finely divided aluminum or beryllium. A suitable binder is incorporated in the propellant composition to bind the individual particles of metal with the particles of oxidizer containing occluded metal.

Shafer, J. I.↗
NASA NTRS1974

Combustion chemistry of solid propellants

Several studies are described of the chemistry of solid propellant combustion which employed a fast-scanning optical spectrometer. Expanded abstracts are presented for four of the studies which were previously reported. One study of the ignition of composite propellants yielded data which suggested early ammonium perchlorate decomposition and reaction. The results of a study of the spatial distribution of molecular species in flames from uncatalyzed and copper or lead catalyzed double-based propellants support previously published conclusions concerning the site of action of these metal catalysts. A study of the ammonium-perchlorate-polymeric-fuel-binder reaction in thin films, made by use of infrared absorption spectrometry, yielded a characterization of a rapid condensed-phase reaction which is likely important during the ignition transient and the burning process.

Baer, A. D.↗
NASA NTRS1977

Electrolytic pretreatment of urine

Electrolysis has been under evaluation for several years as a process to pretreat urine for ultimate recovery of potable water in manned spacecraft applications. The conclusions that were drawn from this investigation are the following: (1) A platinum alloy containing 10 percent rhodium has been shown to be an effective, corrosion-resistant anode material for the electrolytic pretreatment of urine. Black platinum has been found to be suitable as a cathode material. (2) The mechanism of the reactions occurring during the electrolysis of urine is two-stage: (a) a total Kjeldahl nitrogen and total organic carbon (TOC) removal in the first stage is the result of electrochemical oxidation of urea to CO2, H2O, and ammonia followed by chloride interaction to produce N2 from ammonia, (b) after the urea has been essentially removed and the chloride ions have no more ammonia to interact with, the chloride ions start to oxidize to higher valence states, thus producing perchlorates. (3) Formation of perchlorates can be suppressed by high/low current operation, elevated temperature, and pH adjustment. (4) UV-radiation showed promise in assisting electrolytic TOC removal in beaker tests, but was not substantiated in limited single cell testing. This may have been due to non-optimum configurations of the single cell test rig and the light source.

Source record↗
NASA NTRS1979

Alternate propellant program, phase 1

Candidate propellant systems for the shuttle booster solid rocket motor (SRM), which would eliminate, or greatly reduce, the amount of HCl produced in the exhaust of the shuttle SRM were investigated. Ammonium nitrate was selected for consideration as the main oxidizer, with ammonium perchlorate and the nitramine, cyclo-tetramethylene-tetranitramine as secondary oxidizers. The amount of ammonium perchlorate used was limited to an amount which would produce an exhaust containing no more than 3% HCl.

Anderson, F. A.↗
NASA NTRS1981

High temperature propellant development

It is reported that the neccessary technology has been developed and demonstrated for the manufacture of heat-sterilizable solid propellants which meet specific ballistic goals. It is shown that: (1) phosphate doping of ammonium perchlorate significantly enhances the thermal stability of the substance; (2) grinding the ammonium perchlorate to reduce particle size further increases thermal stability; and (3) unsaturated polymers such as the polybutadienes can be successfully used in a heat-sterilizable propellant system. Among the topics considered by the study are oxidizers, dopants, binders, and the thermal cycling of 70 lb and 600 lb propellant grains.

Anderson, F. A.↗
NASA NTRS1993

Release Of Gaseous NH(3) From NH(4)CIO(4) By HTPB-Bonding Agents

Report describes experimental study of rate of generation of ammonia and total amount of ammonia generated by chemical reactions between bonding agents and grains of ammonium perchlorate in solid rocket propellants. Also provides insight into mechanisms of chemical reactions between several types of organic amines with solid ammonium perchlorate.

Mccomb, James C.↗
NASA NTRS1999

The History of Solid-Propellant Rocketry: What We Do and Do Not Know

Contributions to the evolution of solid-propellant rocketry have come from a variety of sources. World War II research on large solids enabled one company to capitalize on work in the area of castable double-base propellants. Separate development of castable composite propellants led to production of Polaris and Minuteman powerplants. Pivotal to the development of these missiles were Edward Hall's advocacy of the Minuteman missile within the Air Force and contract funding to resolve problems. The discovery that adding large amounts of aluminum significantly increased the specific impulse of a castable composite propellant further aided large-missile technology. These separate lines of research led to the development of large solid-propellant motors and boosters. Many more discoveries went into the development of large solid-propellant motors. Ammonium perchlorate replaced potassium perchlorate as an oxidizer in the late 1940's, and binders were developed. Discoveries important in the evolution of large solid-propellant motors appear to have resulted from innovators' education and skills, an exposure to contemporary problems, an awareness of theory but a willingness not to let it dictate empirical investigations, and proper empirical techniques. Other important contributions are the adequate funding and exchange of information. However, many questions remain about these and other innovations.

Hunley, J. D.↗
NASA NTRS2012

A Possible Organic Contribution to the Low Temperature CO2 Release Seen in Mars Phoenix Thermal and Evolved Gas Analyzer Data

Two of the most important discoveries of the Phoenix Mars Lander were the discovery of approx.0.6% perchlorate [1] and 3-5% carbonate [2] in the soils at the landing site in the martian northern plains. The Thermal and Evolved Gas Analyzer (TEGA) instrument was one of the tools that made this discovery. After soil samples were delivered to TEGA and transferred into small ovens, the samples could be heated up to approx.1000 C and the gases that evolved during heating were monitored by a mass spectrometer. A CO2 signal was detected at high temperature (approx.750 C) that has been attributed to calcium carbonate decomposition. In addition to this CO2 release, a lower temperature signal was seen. This lower temperature CO2 release was postulated to be one of three things: 1) desorption of CO2, 2) decomposition of a different carbonate mineral, or 3) CO2 released due to organic combustion. Cannon et al. [3] present another novel hypothesis involving the interaction of decomposition products of a perchlorate salt and calcium carbonate.

Archer, P. D. Jr.↗