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Modified solica spheres enhance chromatographic separation. Commercially available silica spheres are modified by reacting them with molecules containing isocyante and isothiocyanate groups. Applications of surface derivatized spheres that result from reaction include analysis of samples prouced by atmospheric or soil probes.
Several isocyanate and isothiocyanate derivatives Porasil C were synthesized and evaluated for the separation of the low-molecular-weight saturated and unsaturated hydrocarbons. It was shown that different functional groups significantly affect the retention behavior of the more polar unsaturated hydrocarbons, and that reproducible results can be obtained if dry carrier gas is used.
Several isocyanate and isothiocyanate derivatives of Porasil C were synthesized and evaluated for the separation of the low-molecular-weight saturated and unsaturated hydrocarbons. It was shown that different functional groups significantly affect the retention behavior of the more polar unsaturated hydrocarbons, and that reproducible results can be obtained if dry carrier gas is used.
Measurement of the permanent gases in the atmospheres of mission targets is a major objective. A 16 meter long Porapak N column was used on the Venus probe and required a rather high carrier gas flow rate. The researchers have, therefore, surveyed commercial porous polymer types which had some ability to resolve nitrogen, oxygen, argon and carbon monoxide gases. Porapaks N and Q appeared superior to most. Batch to batch variation, however, was quite wide, so the researchers learned how to synthesize porous polymer and investigated some of the factors affecting the separations. A polymer was synthesized which was superior to all commercial products and allowed at least a 50% reduction in length and flow rate of carrier gas. Similar studies were made concerning the separation of hydrocarbons and new porous polymers have been synthesized which represent significant improvements in time of analysis, column, and carrier gas flow rate.
Saponified extracts of rock samples colonized by cryptoendolithic microbial communities from the McMurdo Dry Valleys of Southern Victoria Land, Antarctica, were separated into hydrocarbon and fatty acid fractions by silica gel column chromatography. Hydrocarbons and methyl esters of fatty acids were analyzed by capillary gas chromatography-mass spectrometry. Unusually, a suite of long-chain anteiso-alkanes (a-C20 to a-C30) and anteiso-alkanoic acids (a-C20 to a-C30) were detected in many samples, together with straight-chain, branched and/or cyclic and acyclic isoprenoid compounds. These novel compounds are probably derived from unidentified heterotrophic bacteria or symbiotic processes in a unique microbial community in the Antarctic cold desert and suggest the occurrence of a special biosynthetic pathway. Long-chain anteiso-alkanes are probably formed through microbial decarboxylation of corresponding anteiso-alkanoic acids. They may serve as new biomarkers in environmental and geochemical studies.
Future sustainable energy generation technologies such as photovoltaic and wind farms require advanced energy storage systems on a massive scale to make the alternate (green) energy options practical. The daunting requirements of such large-scale energy systems such as long operating and cycle life, safety, and low cost are not adequately met by state-of-the-art energy storage technologies such as vanadium flow cells, lead-acid, and zinc-bromine batteries. Much attention is being paid to redox batteries specifically to the vanadium redox battery (VRB) due to their simplicity, low cost, and good life characteristics compared to other related battery technologies. NASA is currently seeking high-specific- energy and long-cycle-life rechargeable batteries in the 10-to-100-kW range to support future human exploration missions, such as planetary habitats, human rovers, etc. The flow batteries described above are excellent candidates for these applications, as well as other applications that propose to use regenerative fuel cells. A new flow cell technology is proposed based on coupling two novel electrodes in the form of solvated electron systems (SES) between an alkali (or alkaline earth) metal and poly aromatic hydrocarbons (PAH), separated by an ionically conducting separator. The cell reaction involves the formation of such SES with a PAH of high voltage in the cathode, while the alkali (or alkaline earth metal) is reduced from such an MPAH complex in the anode half-cell. During recharge, the reactions are reversed in both electrodes. In other words, the alkali (alkaline earth) metal ion simply shuttles from one M-PAH complex (SES) to another, which are separated by a metal-ion conducting solid or polymer electrolyte separator. As an example, the concept was demonstrated with Li-naphthalene//Li DDQ (DDQ is 2,3-Dichloro-5,6-dicyano- 1,4-benzoquinone) separated by lithium super ion conductor, either ceramic or polymer (solid polymer or gel polymer) electrolytes. The reactants are Li-naphthalene dissolved in tetrahydrofuran (THF) with a lithium salt of 1M LiBF4 (lithium tetra fluoroborate) in the anode compartment, and DDQ again dissolved in THF and also containing 1M LiBF4 salt in the cathode half-cell. The solid electrolyte separator used in the first set of experiments is a ceramic solid electrolyte, available from a commercial source. The open circuit voltage of the cells is close to 3.0 V, as expected from the individual half-cell voltages of Li-naphthalene and Li-DDQ. Upon discharge, the cell shows steady discharge voltage of 2.7 V, which confirms that the electrochemical processes do involve lithium ion shuttling from the anodic compartment to the cathode half-cell. The reversibility or rechargeability is demonstrated by charging the partially discharged cells (i.e., with lithium present in the DDQ half). Once again, a steady voltage close to 3.0 V was observed during charge, indicating that the system is quite reversible. In the subsequent concept-demonstration studies, the ceramic electrolyte has been replaced with a gel polymer electrolyte, e.g., PVDF-HFP (poly vinylene difluoride hexafluoropropene) gel, which has several advantages such as high ionic conductivity (almost comparable to liquid electrolyte and about 2 orders of magnitude better than the ceramic equivalent), lower cost, and possibly higher chemical stability at the anode. In addition, it can be bonded to the electrode by thermal fusion to form membrane electrode assemblies (MEAs), as is done in fuel cells.
Technique rapid and uses standard analytical equipment. Silane gas containing traces of hydrocarbons injected into carrier gas of moist nitrogen having about 0.2 percent water vapor. Carrier, water and silane pass through short column packed with powdered sodium hydroxide which combines moisture and silane to form nonvolatile sodium silicate. Carrier gas free of silane but containing nonreactive hydrocarbons, pass to silica-gel column where chromatographic separation takes place. Hydrocarbons measured by FID.
A comparison is made between the storable-propellant engine and an equivalent dual-expander engine using oxygen, propane, and hydrogen propellants. The propane and hydrogen dual-expander engine is then compared with previous results with separate propane and hydrocarbon engines. It is shown that the dual-expander reduces vehicle dry mass from 94 to 89 Mg, or 5%. The hydrogen-only thrust of the dual-expander is 0.4 MN, while the separate hydrogen engines have a thrust of 2.3 MN. The low thrust level increases the difficulty of cooling the dual-expander engine, and additional hydrogen flow is added for transpirational cooling. This additional hydrogen flow leads to an increase in the hydrogen tank size. It is also shown that storable propellants increase the dry mass of single-stage earth-to-orbit vehicles by about 20% and the gross mass by about 54%. It is concluded that dual-expander engines should be studied with several thrust splits and thrust levels.
New type of trifunctional alcohol was synthesized from commercially available trimer acid. Trifunctional alcohol is hydrocarbon with widely separated terminal hydroxyl groups, and was expressly developed as crosslinking agent for preparation of polyurethane propellants, binders and case liners.
The behavior of laminar gas jet diffusion flames subjected to elevated gravity in order to investigate the role of buoyancy in such flames has been studied experimentally. Higher than earth normal gravity was achieved using a 1.83 m diameter centrifuge. Methane, ethane, propane and hydrogen air flames were stabilized at the exit of small tubular burners ranging in size from .05 to .21 cm in diameter. The experimental arrangement was such that the flames were burnt vertically upward. Following a shortening of the flame and a decrease in luminosity with increasing gravity level, further increases in gravity caused the hydrocarbon flames to separate from the rim and eventually extinguish. The extinction gravity levels appear to correlate with the parameter g alpha (u)/S to the 3rd (u), which should be a constant for buoyancy controlled extinction. This parameter is developed by a rudimentary analysis of the heat loss from the premixed stabilizing flame in the lifted flame base. When the loss is excessive, the flame is extinguished.
A miniature gas analysis system has been built based on the principles of gas chromatography (GC). The major components are fabricated in silicon using photolithography and chemical etching techniques, which allows size reductions of nearly three orders of magnitude compared to conventional laboratory instruments. The chromatography system consists of a sample injection valve and a 1.5-m-long separating capillary column, which are fabricated on a substrate silicon wafer. The output thermal conductivity detector is separately batch fabricated and integrably mounted on the substrate wafer. The theory of gas chromatography has been used to optimize the performance of the sensor so that separations of gaseous hydrocarbon mixtures are performed in less than 10 s. The system is expected to find application in the areas of portable ambient air quality monitors, implanted biological experiments, and planetary probes.
CFC's and halogenated hydrocarbon solvents have been the solvents of choice to degrease and otherwise clean precision metal parts to allow proper function. Recent regulations have, however, rendered most of these solvents unacceptable for these purposes. New processes which are being used or which have been proposed to replace these solvents usually either fail to remove water soluble contaminants or produce significant aqueous wastes which must then be disposed of. In this work, a new method for cleaning surfaces will be investigated. Solubility of typical contaminants such as lubricating greases and phosphatizing bath residues will be studied in several surfactant/supercritical fluid solutions. The effect of temperature, pressure, and the composition of the cleaning mixture on the solubility of oily, polar, and ionic contaminants will be investigated. A reverse micellar solution in a supercritical light hydrocarbon solvent will be used to clean samples of industrial wastes. A reverse micellar solution is one where water is dissolved into a non-polar solvent with the aid of a surfactant. The solution will be capable of dissolving both water-soluble contaminants and oil soluble contaminants. Once the contaminants have been dissolved into the solution they will be separated from the light hydrocarbon and precipitated by a relatively small pressure drop and the supercritical solvent will be available for recycle for reuse. The process will be compared to the efficacy of supercritical CO2 cleaning by attempting to clean the same types of substrates and machining wastes with the same contaminants using supercritical CO2. It is anticipated that the supercritical CO2 process will not be capable of removing ionic residues.
Gas chromatography test results are presented for two new moderately high-temperature phases of Dexsil 400-GC with free hydroxyl end groups (uncapped) and with end groups covered by trimethyl silyl groups (capped). The two Dexsil 400-GC phases were tested for their ability to resolve N-TFA-DL-(+)-2-butyl esters and n-butyl esters, as well as fatty acid methyl esters and hydrocarbon standards. Generally the more polar uncapped phase was superior to the capped phase in all separation comparisons, except for the hydrocarbons.
Presence of aromatic hydrocarbons in meteorites using chromatographic separation techniques
A routine method was developed to measure benzo(a)pyrene in airborne particulates. Samples were collected on a filter and the organic portion was extracted with cyclohexane. The polynuclear hydrocarbon (PNHC) fraction was separated from the aliphatics by column chromatography. An internal standard was added to the extract and a portion of it was injected into a gas chromatograph. Although the gas chromatographic method has often been reported in the literature, satisfactory separation of benzo(a)pyrene and benzo(e)pyrene has not been achieved. With the introduction of a nematic liquid crystal as the stationary phase good separation is now possible.
A description is presented of a dual-fuel modular split-combustor linear aerospike engine concept. The considered engine represents an approach to an integrated engine for a reusable single-stage-to-orbit (SSTO) vehicle. The engine burns two fuels (hydrogen and a hydrocarbon) with oxygen in separate combustors. Combustion gases expand on a linear aerospike nozzle. An engine preliminary design is discussed. Attention is given to the evaluation process for selecting the optimum number of modules or divisions of the engine, aspects of cooling and power cycle balance, and details of engine operation.
The investigation of the Saturnian System is being proposed jointly by NASA and the European Space Agency (ESA). The mission is scheduled for a launch in 1996. The mission provides an opportunity for close observation and exploration of Saturn's atmosphere, the complex Saturnian System of satellites and rings, Titan (Saturn's planet-sized moon), and Saturn's magnetosphere. The mission gives special attention to Titan which is blanketed by a thick, opaque atmosphere. An atmospheric probe will be deposited into the Titan Atmosphere for in situ measurement during a slow, three hour descent to the surface. The results from this analysis may provide the information which is important to the research of chemical evolution, and the origin of life. An analytical system was developed as a part of the Titan Aerosol Gas Experiment (TAGEX), a proposed experiment for the Cassini Mission. This system will use two highly sensitive detectors, the Metastable Ionization Detector (MID) and the Ion Mobility Spectrometer (IMS). Unfortunately, when commercial columns are utilized with these highly sensitive detectors, volatile components continuously bleed from the column and interfere with the detector. In addition, light columns must be able to separate polar and nonpolar organic chemicals within 10-15 minutes under isothermal conditions for the Titan Mission. Therefore, a highly crosslinked silicone polymeric packed column was developed which is able to efficiently separate amines, alcohols, and hydrocarbons with retention times less that 15 minutes at 100 C isothermal condition.
As early as 1937 German scientists at Peenemunde experimented with highly unstable fuel blends of nitrous oxide (N2O) and ethanol. These early tests mostly resulted in explosions and destroyed rocket engines. More recently several companies have developed experimental nitrous oxide fuel blends (NOFB) with Isp exceeding 300 sec. Although NOFBx has recently been cleared for tests on the International Space Station, this propellant remains highly experimental and has not been cleared for commercial transport by the US DOT. Recent work by Karabeyoglu et al. has raised concerns about the safety risks of mixing hydrocarbons with N2O. Liquid oxidizer/fuel blends are highly explosive and require extreme care in transport and servicing. By adding small amounts of a liquid organic fuel such as alcohol or a hydrocarbon, the odds of an explosive decomposition event are significantly increased.iv The proposed solution mitigates the explosion hazards of NOFB by separating the oxidizer from the hydrocarbon fuel formed as of a small cylindrical section of ABS thermoplastic. As N2O vapor flows across the grain segment, current enters a 1000 VDC high-tension lead in the ABS fuel grain and produces an inductive spark that vaporizes a small amount of the material. The ablated fuel vapor plus residual energy from the spark seed a localized exothermic N2O dissociation that produces sufficient heat to initiate combustion. The process is also effective when gaseous oxygen is used. A low TRL (2-3) prototype demonstrating the feasibility of controlled hydrocarbon-seeding was recently tested at Utah State University.v The unit features a miniature 2.5 cm ABS fuel grain fabricated using a Stratasys Dimension 3-D printer. The 9-N thruster was pulse-fired up to 27 consecutive times on a single ABS grain segment. Ignition was achieved by as little as 12-15 Joules energy input. This value is contrasted with the typical 30-minute pre-heat requirement for the ECAPS LMP-103S ADN-based monopropellant, requiring an energy input of 14,850 Joules for catalytic dissociation. The hydrocarbon-seeded micro-hybrid was also adapted as a non-pyrotechnic ignitor for a 900 N (200-lbf) thrust hybrid motor. The motor was successfully ignited 4 consecutive times with no hardware swaps or propellant additions. The amount of ABS seed material that can be fit into the injector cap is the only limit to the number of available repeat firings. This series of tests marks the first time a hybrid motor was ever ignited by other than a solid-propellant pyrotechnic charge or bi-propellant flame ignitor. Nitrous oxide hybrid motors are typically difficult to ignite and usually require multiple solid-propellant charges to initiate combustion, so this nonpyrotechnic ignition is a significant accomplishment. The controlled hydrocarbon-seeding approach is fundamentally different from all other green propellant solutions offered by the aerospace industry. Although the proposed system is more correctly a hybrid technology; the system retains all the simple features of a monopropellant design. To date no optimization study has been performed to identify the best grain geometry for electrostatic ignition. Fortunately, because the grain segments are fabricated using rapid-prototyping technology, changing the grain geometry is as simple as modifying the 3-D printer CAD-file. Vacuum Isp exceeding 270 seconds has been demonstrated (Ref v), a value significantly higher than those offered by competing green monopropellant options. The propellants of choice, N2O/GOX and ABS are 100% non-toxic, non-explosive, and environmentally benign. Because the inert oxidizer and fuel components are mixed only within the combustion chamber, the system retains the inherent safety of a hybrid rocket and can be piggy-backed as a secondary payload with no overall mission risk increase to the primary payload, an excellent characteristic for secondary launch systems.