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NASA NTRS1979

Characterization of the adsorption of water vapor and chlorine on microcrystalline silica

The characterization of water adsorption on silica is necessary to an understanding of how hydrogen chloride interacts with silica. The adsorption as a function of outgas temperatures of silica and as a function of the isotherm temperature was studied. Characterization of the silica structure by infrared analysis, X-ray diffraction and differential scanning calorimetry, surface area determinations, characterization of the sample surface by electron spectroscopy for chemical analysis (ESCA), and determinations of the heat of immersion in water of silica were investigated. The silica with a scanning electron microscope was examined.

Skiles, J. A.↗

NASA NTRS1988

A diffuse reflectance infrared Fourier transform spectroscopic study of adsorbed hydrazines

Diffuse reflectance spectroscopy of fuel hydrazines adsorbed on silica, silica-alumina and alimina surfaces indicates that the primary surface-hydrazine interaction is hydrogen bonding. Hydrazine, on adsorption to a deuterated silica surface, undergoes a rapid H/D exchange with deuterated surface silanol (Si-OD) groups. Adsorption equilibria are rapidly established at room temperature. Monomethylhydrazine and unsymmetrical dimethylhydrazine are similarly adsorbed. On adsorption, the C-H stretching and methyl deformation modes of the methylhydrazines are shifted to higher frequencies by 10 to 20 cm(-1). These shifts are postulated to be due to changes in the lone-pair electro-density on the adjacent nitrogen atom and an electronegativity effect.

Davis, Dennis D.↗

NASA NTRS1975

Electrochemical generation of oxygen. 1: The effects of anions and cations on hydrogen chemisorption and anodic oxide film formation on platinum electrode. 2: The effects of anions and cations on oxygen generation on platinum electrode

The effects were studied of anions and cations on hydrogen chemisorption and anodic oxide film formation on Pt by linear sweep voltammetry, and on oxygen generation on Pt by potentiostatic overpotential measurement. The hydrogen chemisorption and anodic oxide film formation regions are greatly influenced by anion adsorption. In acids, the strongly bound hydrogen occurs at more cathodic potential when chloride and sulfate are present. Sulfate affects the initial phase of oxide film formation by produced fine structure while chloride retards the oxide-film formation. In alkaline solutions, both strongly and weakly bound hydrogen are influenced by iodide, cyanide, and barium and calcium cations. These ions also influence the oxide film formation. Factors considered to explain these effects are discussed. The Tafel slope for oxygen generation was found to be independent on the oxide thickness and the presence of cations or anions. The catalytic activity indicated by the exchange current density was observed decreasing with increasing oxide layer thickness, only a minor dependence on the addition of certain cations and anions was found.

Huang, C. J.↗

NASA NTRS1972

Some surface characteristics and gas interactions of Apollo 14 fines and rock fragments.

Comprehensive survey of the physical surface characteristics of Apollo 14 fines, two fragments of a breccia (14321), and a crystalline rock (14310). The survey was carried out with optical and both scanning and transmission electron microscopy and by studying the adsorption of a variety of gases including nitrogen, hydrogen, and water vapor. Our objective in the optical microscope study was to relate the visible geological and petrological features to the surface properties. Electron microscopy particularly helped relate surface roughness and particle fusion to gas adsorption and pore structure. The fine sample (14163,111) had a surface area of 0.210 sq m/g and a helium density of 2.9 g/cc. Similar values have been observed with breccia fragments. Other observations include physical adsorption of molecular hydrogen at low temperatures and of water vapor at ambient temperatures. It is concluded that these particular lunar materials, while capable of adsorbing water vapor, do not retain it for any significant time at low pressures, nor, under lunar conditions, is there any indication of absorption or penetration.

Cadenhead, D. A.↗

NASA NTRS1981

Possible selective adsorption of enantiomers by Na-montmorillonite

Racemic amino acids including (D,L) alpha-alamine, (D,L) alpha-aminobutyric acid, (D,L) valine, and (D,L) norvaline were incubated with Na-montmorillonite at 100% CEC at three hydrogen ion concentrations, and amino acid adsorption was determined by ion exchange chromatography. Enantiomers were analyzed by gas chromatography. Differences in the quantities of D and L enantiomers in any of the fractions was no larger than a few percent. Although a large difference in the adsorption of the amino acid enantiomers was not observed, the analysis may indicate a small preferential adsorption (0.5-2%) of L-amino acids by Na-montmorillonite.

Friebele, E.↗

NASA NTRS1975

Chemisorption kinetics of hydrogen on evaporated iron films

Measurements were made of the isothermal adsorption-desorption kinetics for H2 chemisorbed onto Fe films. The chemisorption process is observed to proceed via a precursor state of adsorbed molecular hydrogen similar to the H2-Ni system. The first measurements of the activation energy for desorption, and estimates of the values of the fast kinetic rates between the precursor and chemisorbed states are reported. Adsorption into the precursor state does not appear to be activated, but the process connecting the precursor state with the chemisorbed state will, under certain circumstances, be a rate limiting step for adsorption. The effects of contamination of the surface are evidenced in the measurements.

Shanabarger, M. R.↗

NASA NTRSDate not supplied

Evaluation of Low-Energy Hydrogen Separation Method Using Metal-Organic Frameworks (MOFs) for Closed-Loop ECLSS Air Revitalization (CLEAR)

The State-of-the-Art (SOA) air revitalization architecture onboard the International Space Station (ISS) recovered approximately 50% of the oxygen (O 2 ) from metabolic carbon dioxide (CO 2 ) via the Sabatier process from 2011 to 2017. O 2 recovery is currently constrained by the limited availability of reactant hydrogen (H 2 ) preventing complete conversion of CO 2 to H 2 O. Increasing O 2 recovery within Closed-Loop ECLSS is essential to reducing resupply mass for long-duration manned missions; specifically focusing on water (H 2 O) which supplies H 2 for Sabatier via water electrolysis. Past ground test endeavors at Marshall Space Flight Center (MSFC) have attempted to recover H 2 from Sabatier-produced CH 4 using technologies such as carbon vapor deposition (CVD) and plasma pyrolysis. The byproducts of these technologies can act as a catalyst poison or reactor deadload to the Sabatier reactor. Hydrogen separation techniques must be utilized to maintain the Sabatier catalyst during gas recycling and must be scalable, non-energy intensive, and safe to operate in a habitation setting. Research indicated that metal-organic frameworks (MOFs) could meet these criteria and were tested for their capability to capture the various carbon-based gaseous products of CVD and plasma pyrolysis such as acetylene (C 2 H 2 ), ethylene (C 2 H 4 ), ethane (C 2 H 6 ), and carbon monoxide (CO) which would purify the hydrogen gas stream passing through the MOF. A sub-scale adsorption column was developed by Marshall Space Flight Center to test three MOF candidates against a synthetic gas mixture comprised of process-relevant carbonous gases and hydrogen to evaluate the separation capability of the MOFs. The results of the hydrogen separation capability, isothermal desorption capability, and demonstrated cyclic reuse of the MOF are presented in this paper.

Kagen Crawford↗

NASA NTRS1973

Solar wind and terrestrial atmosphere effects on lunar sample surface composition

Samples returned from the Apollo missions have been shown to have undergone a partial surface oxidation with the degree of oxidation being dependent on the intensity and duration of exposure to a terrestrial or other oxidizing atmosphere. Exposure to atomic hydrogen at room temperature, or molecular hydrogen above 100 C results in a surface reduction. The adsorption of water vapor on a test sample was found to be only slightly dependent on the state of surface oxidation, a situation consistent with the formation of hydroxyl groups on the surface when a sample is exposed to hydrogen. That hydroxyl groups are indeed formed is substantiated by the release of water vapor (and by release of heavy water following exposure to deuterium), indicating that water vapor can be synthesized from solar wind hydrogen and sample oxygen. Observations of trace amounts of methane indicate that the reduction process is by no means restricted to the formation of water vapor.

Cadenhead, D. A.↗

NASA NTRS1964

Some Theoretical Aspect of Cryosorption

When a gas or vapor is allowed to come to equilibrium with a solid surface, the concentration of gas molecules is always found to be greater in the immediate vicinity of the surface than in the free gas phase, regardless of the nature of the gas or of the surface. The process by which this surface excess is formed is termed adsorption. In any solid, the atoms at the surface are subject to unbalanced forces of attraction normal to the surface plane; the balance of forces is partially restored by the adsorption of gas molecules. If the forces responsible for adsorption are of van der Waals type, the process is called physical adsorption. Furthermore, if the solid (and its surface) are maintained at relatively low temperatures (say 50°K or below), the term cryosorption is used.

ADSORPTION↗

NASA NTRS1975

Interaction of hydrogen chloride with alumina

The influence of outgas conditions and temperature on the adsorptive properties of two aluminas Alon-c and Al6sG were studied using adsorption isotherm measurements. Alon-C and Al6SG were characterized using X-ray powder diffraction, thermogravimetric analysis (TGA), scanning electron microscopy (SEM) and BET nitrogen surface areas. Some of these techniques were applied to two other aluminas but no isotherm data was obtained. Isotherm data and techniques applied to each alumina are summarized in tabular form.

Bailey, R. R.↗

NASA NTRSDate not supplied

Simulation of Acetylene Adsorption Columns for Regenerative Life Support Systems

In oxygen recovery systems using Sabatier reactors, hydrogen (H 2 ) is the limiting factor in the Sabatier reaction. Aboard the International Space Station, electrolysis of water produces H 2 . However, additional H 2 can be provided by plasma pyrolysis of hydrocarbons, increasing the amount of H 2 available to the Sabatier reaction.

Regenerative Life Support↗

NASA NTRS1988

Short-Cycle Adsorption Refrigerator

Modular adsorption/Joule-Thomson-effect refrigerator offers fast regeneration; adsorption/desorption cycle time expected to be 1 minute. Pressurized hydrogen generated by bank of compressor modules during heating phase passes through system of check valves and expands in Joule-Thomson junction as it enters refrigeration chamber. Hydrogen absorbs heat from load before it is sucked out by another bank of compressor modules in cooling phase.

Chan, C. K.↗

NASA NTRS1990

Surface characterization of hydrogen charged and uncharged alpha-2 and gamma titanium aluminide alloys using AES and REELS

The surfaces of selected uncharged and hydrogen charged alpha-2 and gamma titanium aluminide alloys with Nb additions were characterized by Auger electron (AES) and reflected electron energy loss (REELS) spectroscopy. The alloy surfaces were cleaned before analysis at room temperature by ion sputtering. The low energy (500 eV) ion sputtering process preferentially sputtered the surface concentration. The surface concentrations were determined by comparing AES data from the alloys with corresponding data from elemental references. No differences were observed in the Ti or Nb Auger spectra for the uncharged and hydrogen charged alloys, even though the alpha-2 alloy had 33.4 atomic percent dissolved hydrogen. Also, no differences were observed in the AES spectra when hydrogen was adsorbed from the gas phase. Bulk plasmon energy shifts were observed in all alloys. The energy shifts were induced either by dissolved hydrogen (alpha-2 alloy) or hydrogen adsorbed from the gas phase (alpha-2 and gamma alloys). The adsorption induced plasmon energy shifts were greatest for the gamma alloy and cp-Ti metal.

Shanabarger, M. R.↗

NASA NTRS1973

The catalytic removal of ammonia and nitrogen oxides from spacecabin atmospheres

Investigations were made on methods for the removal of ammonia and to a lesser extent nitrogen oxides in low concentrations from air. The catalytic oxidation of ammonia was studied over a temperature range of 250 F to 600 F and a concentration range 20 ppm to 500 ppm. Of the catalysts studied, 0.5 percent ruthenium supported on alumina was found to be superior. This material is active at temperatures as low as 250 F and was found to produce much less nitrous oxide than the other two active catalysts, platinum on alumina and Hopcalite. A quantitative design model was developed which will permit the performance of an oxidizer to be calculated. The ruthenium was found to be relatively insensitive to low concentrations of water and to oxygen concentration between 21 percent and 100 percent. Hydrogen sulfide was found to be a poison when injected in relatively large quantities. The adsorption of ammonia by copper sulfate treated silica gel was investigated at temperatures of 72 F and 100 F. A quantitative model was developed for predicting adsorption bed behavior.

Gully, A. J.↗

NASA NTRSDate not supplied

Experimental Results of a Rapidly Cycled Temperature Swing Adsorption Pump in a Terrestrial Environment

To improve the increasing CO 2 levels on Earth, technology for carbon capture and utilization must be efficient and cost effective. One major contributor of atmospheric CO 2 is post-combustion flue gas, which can contain up to 20% CO 2 . Scrubbing this CO 2 could reduce the environmental impact of this common industrial process. In off-Earth environments, capturing and utilizing CO 2 from space resources is useful for crewed spaceflight life support. Specifically, the Bosch process, which produces water and carbon powder by reacting CO 2 and hydrogen, is a possible in-situ resource utilization (ISRU) architecture for the Moon and Mars. The Rapid Cycle Temperature Swing Adsorption (RC-TSA) pump is an innovative technology designed to capture CO 2 efficiently. The RC-TSA leverages a stacked plate geometry to cycle multiple zeolite-coated beds. The thin layers allow for rapid heat transfer of the zeolite coating, which improves performance over previously tested pump designs. The design is favorable for scalability and manufacturability, which are forward work. Initial testing of the sorption pump using a simulated flue gas environment shows favorable breakthrough capacities and reduced cycle times. Results show promise for on- and off-Earth applications, such as a Martian surface and crewed spaceflight environments.

adsorption pump↗

NASA NTRS1972

Catalysts for initiating the hydrogen-oxygen reaction at 78 K.

Catalysts for initiating reaction of hydrogen with oxygen in gas mixtures at temperatures down to 78 K (-195 C) were sought. A rising-temperature reactor was used for detecting onset of reaction. The platinum metals, especially iridium, platinum, and ruthenium, were the most active. With high concentrations of iridium on an alumina support, reaction initiation was observed at -195 C for a helium stream containing 3% hydrogen and 1% oxygen. Best results were obtained when the catalyst had been preheated in hydrogen and cooled in a hydrogen environment before being contacted with oxygen-containing gas. The initiation is interpreted to be the result of transient phenomena which occur when a hydrogen-oxygen mixture contacts an active catalyst. Chemisorption of oxygen and formation of some water, along with water adsorption on the support, serve to raise the temperature to a point where true catalysis can proceed.

Jennings, T. J.↗

NASA NTRS1973

Ultrafiltration by a compacted clay membrane. I - Oxygen and hydrogen isotopic fractionation. II - Sodium ion exclusion at various ionic strengths.

Laboratory experiments were carried out to determine the magnitude of the isotopic fractionation of distilled water and of 0.01N NaCl forced to flow at ambient temperature under a hydraulic pressure drop of 100 bars across a montmorillonite disk compacted to a porosity of 35% by a pressure of 330 bars. The ultrafiltrates in both experiments were depleted in D by 2.5% and in O-18 by 0.8% relative to the residual solution. No additional isotopic fractionation due to a salt-filtering mechanism was observed at NaCl concentrations up to 0.01N. Adsorption is most likely the principal mechanism which produces isotopic fractionation, but molecular diffusion may play a minor role. The results suggest that oxygen and hydrogen isotopic fractionation of ground water during passage through compacted clayey sediments should be a common occurrence, in accord with published interpretations of isotopic data from the Illinois and Alberta basins. It is shown how it is possible to proceed from the ion exchange capacity of clay minerals and, by means of the Donnan membrane equilibrium concept and the Teorell-Meyer-Siever theory, develop a theory to explain why and to what extent ultrafiltration occurs when solutions of known concentration are forced to flow through a clay membrane.

Coplen, T. B.↗

NASA NTRS2012

Fischer-Tropsch Cobalt Catalyst Improvements with the Presence of TiO2, La2O3, and ZrO2 on an Alumina Support

The objective of this study was to evaluate the effect of titanium oxide, lanthanum oxide, and zirconium oxide on alumina supported cobalt catalysts. The hypothesis was that the presence of lanthanum oxide, titanium oxide, and zirconium oxide would reduce the interaction between cobalt and the alumina support. This was of interest because an optimized weakened interaction could lead to the most advantageous cobalt dispersion, particle size, and reducibility. The presence of these oxides on the support were investigated using a wide range of characterization techniques such as SEM, nitrogen adsorption, x-ray diffraction (XRD), temperature programmed reduction (TPR), temperature programmed reduction after reduction (TPR-AR), and hydrogen chemisorptions/pulse reoxidation. Results indicated that both La2O3 and TiO2 doped supports facilitated the reduction of cobalt oxide species in reference to pure alumina supported cobalt catalysts, however further investigation is needed to determine the effect of ZrO2 on the reduction profile. Results showed an increased corrected cluster size for all three doped supported catalysts in comparison to their reference catalysts. The increase in reduction and an increase in the cluster size led to the conclusion that the support-metal interaction weakened by the addition of TiO2 and La2O3. It is also likely that the interaction decreased upon presence of ZrO2 on the alumina, but further research is necessary. Preliminary results have indicated that the alumina-supported catalysts with titanium oxide and lanthanum oxide present are of interest because of the weakened cobalt support interaction. These catalysts showed an increased extent of reduction, therefore more metallic cobalt is present on the support. However, whether or not there is more cobalt available to participate in the Fischer-Tropsch synthesis reaction (cobalt surface atoms) depends also on the cluster size. On one hand, increasing cluster size alone tends to decrease the active site density; on the other hand, by increasing the size of the cobalt clusters, there is less likelihood of forming oxidized cobalt complexes (cobalt aluminate) during Fischer-Tropsch synthesis. Thus, from the standpoint of stability, improving the extent of reduction while increasing the particle size slightly may be beneficial for maintaining the sites, even if there is a slight decrease in overall initial active site density.

Klettlinger, Jennifer Lindsey Suder↗