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NASA NTRS1976

Functional colloidal particles for immunoresearch

The paper deals with the development of a new class of immunological reagents consisting of antibodies covalently bonded to polymeric microspheres to serve as convenient markers for detection of cell surface antigens by scanning electron and light microscopy. Attention is focused on the design and synthesis of spherical particles containing hydroxyl and carboxyl groups on their surface in a wide range of sizes (30-340 nm diam) by emulsion copolymerization, the preparation of spherical particles ranging from 300 nm to 3 microns and containing a variety of functional groups by means of ionizing radiation, and the experimental conditions for the covalent bonding of fluorescent molecules and antibodies to the spheres by means of the cyanogen bromide, carbodiimide and glutaraldehyde methods. These reagents are used to locate antigens on red blood cells, on mouse and human lymphocytes, and on the surface of photoreceptors. They offer a number of advantages and applications for the study of cell surfaces for immunodiagnosis.

Yen, S. P. S.↗

NASA NTRS1978

Measurement of total organic concentration in water

Instrument for determining total organic concentration in water uses no corrosive reagents or gases. Instead continuous ultraviolet photolysis process converts organic compounds to carbon dioxide (CO2). CO2 electrode is used to measure CO2 content. Only reagent necessary is oxygen, generated in situ by electrolyzing some water. In addition to application in aerospace industry, system has potential uses in pollution monitoring and in laboratory analyses.

Winkler, E.↗

NASA NTRS1979

Overview of methods for extraterrestrial materials processing

A brief survey of processing systems suitable for conversion of lunar soil fractions to refined industrial feedstocks are given. Description of a 'baseline' process using hydrochemical or metallurgical separation of compounds of major and minor elements using HF acid leaching as the initial step is presented. Rough engineering parameters including power and heat rejection requirements, potential loss of earth supplied reagents during recycling, and mass: output ratios of equipment, reagent inventory, and associated power and radiator facilities are described. Minimal practical scales for such systems and manpower requirements are discussed.

Waldron, R. D.↗

NASA NTRS1980

Silicon halide-alkali metal flames as a source of solar grade silicon

The feasibility of using continuous high-temperature reactions of alkali metals and silicon halides to produce silicon in large quantities and of suitable purity for use in the production of photovoltaic solar cells was demonstrated. Low pressure experiments were performed demonstrating the production of free silicon and providing experience with the construction of reactant vapor generators. Further experiments at higher reagent flow rates were performed in a low temperature flow tube configuration with co-axial injection of reagents and relatively pure silicon was produced. A high temperature graphite flow tube was built and continuous separation of Si from NaCl was demonstrated. A larger scaled well stirred reactor was built. Experiments were performed to investigate the compatability of graphite based reactor materials of construction with sodium. At 1100 to 1200 K none of these materials were found to be suitable. At 1700 K the graphites performed well with little damage except to coatings of pyrolytic graphite and silicon carbide which were damaged.

Olson, D. B.↗

NASA NTRS1976

Research in acetylene containing monomers

The preparation of precursor bisbenzils with pendant acetylene linkages for use in the synthesis of new aromatic poly (phenyl quinoxalines) was investigated. Attempts to condense para, para prime-dibromo benzil and potassium acetylide in liquid ammonia and in toluene, to prepare 4-phenyl acetyl phenyl ether, 4-(paraacetylphenyl) acetyl phenyl ether, 4-phenyl acetyl-4 primeacetyl phenyl acetyl phenyl ether, the reaction of 4-phenyl acetyl phenyl ether with Villsmeier reagent to prepare 4-(beta-chloro cinnamaldehyde) phenyl ether, the reaction of 4-(para-acetyl phenyl) acetyl phenyl ether with Villsmeier reagent, and the oxidation of bibenzil to prepare benzil are described. The reactions of phenyl acetylene with oxidizing agent, of phenyl acetylene with bromine, of 1,1,2,2-tetrabromo ethyl benzene with zinc and with oxidizing agent are described.

Ogliaruso, M. A.↗

NASA NTRS1982

Method of neutralizing the corrosive surface of amine-cured epoxy resins

The corrosive alkaline surface layer of an epoxy resin product formed by the curing of the epoxy with an aliphatic amine is eliminated by first applying a non-solvent to remove most or all of the free unreacted amine and then applying a layer of a chemical reagent to neutralize the unused amine or amine functional groups by forming a substituted urea. The surface then may be rinsed with acetone and then with alcohol. The non-solvent may be an alcohol. The neutralizing chemical reagent is a mono-isocyanate or a mono-isothiocyanate. Preferred is an aromatic mono-isocyanate such as phenyl isocyanate, nitrophenyl isocyanate and naplthyl isocyanate.

Lee, S. Y.↗

NASA NTRS1986

Tropospheric HO2 determination by FAGE

The detection efficiency is greatest at low pressures, where the subsequent removal of the HO product by the NO reagent (via HO + NO + M yields HONO + M) is relatively slow. Moreover, nozzle expansion of the air from ambient to low pressures produces a turbulent zone that assists in mixing the reagent with the sample. If the HO product is observed by laser-excited fluorescence, then the other advantages of low-pressure detection by FAGE (Fluorescence Assay with Gas Expansion) also apply. The FAGE instrumental response was calibrated to external HO2 by observing NO decay in the photolysis of HO-CH2O mixtures and by choosing conditions in which HO2 + NO is the only significant NO destruction path. HO2 was determined in urban air.

Obrien, R. J.↗

NASA NTRS1988

Deuterium exchange during acid-demineralisation

Isotopic analyses of residues prepared by demineralization of the Murchison meteorite using D-labelled reagents provide evidence for measurable exchange of H-isotopes between residue and reagents. Precise quantification of this effect is precluded by substantial inhomogeneity of the meteoritic organic matter. A conservative estimate of the degree of exchange is 3-5 percent of the H pyrolyzable as H2O. This could affect the shape of the curve defining D release as a function of temperature, but does not change conclusions previously drawn concerning the nature of the bulk D enrichment of insoluble organic matter in meteorites.

Kerridge, John F.↗

NASA NTRS1990

Prepenetrant Etchant For Incology(R) 903 Weld Overlays

Etching solution developed for use prior to type-IVc penetrant inspection of Incology(R) 903 weld overlays. Formulated as follows: 80 g ferric chloride hexahydrate, 300 mL reagent-grade hydrochloric acid, 25 mL food- or reagent-grade phosphoric acid, and 100 mL ethylene glycol. Gives more reasonable range of etching time and reduces probability of overetching and resulting damage. Stored indefinitely.

O'Tousa, Joseph E.↗

NASA NTRS1990

Lunar oxygen and metal for use in near-Earth space: Magma electrolysis

Because it is energetically easier to get material from the Moon to Earth orbit than from the Earth itself, the Moon is a potentially valuable source of materials for use in space. The unique conditions on the Moon, such as vacuum, absence of many reagents common on the Earth, and the presence of very nontraditional ores suggest that a unique and nontraditional process for extracting materials from the ores may prove the most practical. With this in mind, an investigation of unfluxed silicate electrolysis as a method for extracting oxygen, iron, and silicon from lunar regolith was initiated and is discussed. The advantages of the process include simplicity of concept, absence of need to supply reagents from Earth, and low power and mass requirements for the processing plant. Disadvantages include the need for uninterrupted high temperature and the highly corrosive nature of the high-temperature silicate melts which has made identifying suitable electrode and container materials difficult.

Colson, Russell O.↗

NASA NTRS1990

Lunar oxygen and metal for use in near-earth space - Magma electrolysis

The unique conditions on the moon, such as vacuum, absence of many reagents common on the earth, and presence of very nontraditional 'ores', suggest that a unique and nontraditional process for extracting materials from the ores may prove the most practical. An investigation has begun into unfluxed silicate electrolysis as a method for extracting oxygen, Fe, and Si from lunar regolith. The advantages of the process include simplicity of concept, absence of need to supply reagents from the earth, and low power and mass requirements for the processing plant. Disadvantages include the need for uninterrupted high temperature and the highly corrosive nature of the high-temperature silicate melts, which has made identifying suitable electrode and container materials difficult.

Colson, Russell O.↗

NASA NTRS1992

FAGE measurements of tropospheric HO with measurements and model of interferences

Ambient HO measurements by low-pressure laser-excited fluorescence with chemical modulation, and supporting ozone and water-vapor data, are presented for periods in May and August 1987. The observed peak daytime ambient HO concentrations are in the range (2.5 to 8) x 10 exp 6 molecules/cu cm and show small negative offsets due to photochemical interference. Direct measurements of the interference at fixed (O3) give the dependence on ambient (H2O) and on the modulating reagent (isobutane). At ambient (O3) = 30 ppb and 10 torr H2O, with excitation and detection at a total pressure of 4 torr, the net interference is equal to (HO) = -1.3 x 10 exp 6 molecules/cu cm. Production of HO by the reaction of isobutane with O(1D) accounts for the negative interference. Quenching of HO fluorescence by the modulating reagent contributes a smaller positive term to the interference; kinetic measurements of the quenching rate coefficient are reported. The experimental interference results are compared with a detailed kinetic model of HO production, excitation, relaxation, and detection; reasonable agreement is found.

Hard, T. M.↗

NASA NTRS1994

Tropospheric HO determination by FAGE

In the measurement of tropospheric HO we have employed three low-pressure laser-excited fluorescence (LEF) experimental systems. These instruments operate by expanding the ambient air flow via a nozzle, followed by transit down a flowtube through a detection region traversed by the excitation laser beam. This sampling method we named FAGE (fluorescence assay with gas expansion). The instruments employed a hydrocarbon reagent, added below the nozzle, to remove HO for background measurement. In the second and third instruments, air sampling via parallel nozzles and tubes, with reagent addition alternating between two channels, permitted continuous signal measurement with simultaneous measurement of background. The first two instruments (FAGE1 and FAGE2) used 282 nm HO excitation by frequency-doubled tunable dye lasers, pumped by pulsed Nd:YAG lasers at 10-30 Hz repetition rate. The third instrument (FAGE3) uses 308 nm excitation in which the dye laser is pumped by a copper vapor laser, pulsed at 5600 Hz.

Hard, Thomas M.↗

NASA NTRS1994

Mars aqueous chemistry experiment

Mars Aqueous Chemistry Experiment (MACE) is designed to conduct a variety of measurements on regolith samples, encompassing mineral phase analyses, chemical interactions with H2O, and physical properties determinations. From these data, much can be learned or inferred regarding the past weathering environment, the contemporaneous soil micro-environments, and the general chemical and physical state of the Martian regolith. By analyzing both soil and duricrust samples, the nature of the latter may become more apparent. Sites may be characterized for comparative purposes and criteria could be set for selection of high priority materials on future sample return missions. The second year of the MACE project has shown significant progress in two major areas. MACE Instrument concept definition is a baseline design that has been generated for the complete MACE instrument, including definition of analysis modes, mass estimates and thermal model. The design includes multiple reagent reservoirs, 10 discrete analysis cells, sample manipulation capability, and thermal control. The MACE Measurement subsystems development progress is reported regarding measurement capabilities for aqueous ion sensing, evolved gas sensing, solution conductivity measurement, reagent addition (titration) capabilities, and optical sensing of suspended particles.

Clark, Benton C.↗

NASA NTRS1995

Mars Aqueous Chemistry Experiment (MACE)

The concept of an aqueous-based chemical analyzer for Martian surface materials has been demonstrated to be feasible. During the processes of analysis, design, breadboarding, and most importantly, testing, it has become quite apparent that there are many challenges in implementing such a system. Nonetheless, excellent progress has been made and a number of problems which arose have been solved. The ability to conduct this work under a development environment which is separate and which precedes the project-level development has allowed us to find solutions to these implementation realities at low cost. If the instrument had been selected for a mission without this laboratory pre-project work, the costs of implementation would be much higher. In the four areas covered in Sections D, E, F, and G of this Final Report, outstanding progress has been made. There still remains the task of flight-qualifying certain of the components. This is traditionally done under the aegis of a Flight Project, but just as the concept development can be done at much lower cost when kept small and focused, so could the qualification program of critical parts benefit. We recommend, therefore, that NASA consider means of such qualifications and brass-boarding, in advance of final flight development. This is a generic recommendation, but hardware such as the Mars aqueous chemistry experiment (MACE) and other similarly-new concepts are particularly applicable. MACE now has wide versatility, in being able to reliably dispense both liquids and solids as chemical reagents to an entire suite of samples. The hardware and the experiment is much simpler than was developed for the Viking Biology instrument, yet can accomplish all the inorganic chemical measurements that the Viking desing was capable of. In addition, it is much more flexible and versatile to new experiment protocols (and reagents) than the Viking design ever could have been. MACE opens up the opportunity for many different scientific disciplines to design sub- experiments and to benefit from the investigations that can be conducted. In this sense, it will have the value of a facility, although our recommendation would be that it be under the stewardship of a single lead investigator to insure that conflicting requirements not compromise the straight-forward design that have been achieved. MACE is an excellent candidate for upcoming Mars missions, including the Mars Surveyor Program (MSP) lander missions in 2001 and 2003. In addition, it could be used for any mission to the surface of any other planet or planetary body (including small bodies). An important next step is to encourage various investigators to propose specific uses for this experiment that specifically address their major scientific objectives for upcoming missions.

Benton, Clark C.↗

NASA NTRS1998

Mars Molecular and Isotopic Analysis Research Study

Recently, the Martian atmosphere and surface constituents have become of great interest. The Viking in situ gas chromatograph mass spectrometer experiment contributed greatly to our knowledge of the composition of the Martian atmosphere. However, important questions remain such as the abundance of water on Mars. The Viking experiment employed solid reagents to enhance their carbon measurements. Techniques of chemical conversion using simple solid reagents have advanced considerably in the past 20 years. In this investigation we researched the advancements in techniques to reversibly adsorb and desorb water and focused on the techniques potentially useful for the temperatures and pressures on the Martian surface. During the granting period from June 15, 1998 to August 14, 1998, a literature study of the material appropriate for use in a chemical conversion device and the availability of these materials were undertaken. The focus of this investigation was searching for methods and materials potentially useful in enhancing the measurements of water. Three different methods were considered for the means to extract water from a given gas sample. These methods included adsorption in a desiccant, adsorption on a clean metal surface, and adsorption in a carbon molecular sieve or zeolite. Each method was evaluated with feasibility and reversibility in mind. By far the simplest and perhaps cheapest way to remove water from a gaseous sample is by means of a bulk desiccant. Desiccants are commercially available from many companies including those that supply chemicals. The main feature of a desiccant is its ability to rapidly bind or absorb water from the atmosphere. Calcium chloride, for example, is frequently incorporated into drying tubes by organic chemists when reactions require the absence of water. Other desiccants include sodium hydroxide, calcium hydride, and commercial products such as Drierite, available from Aldrich Chemical. The disadvantage to most desiccants is a direct consequence of what makes them so advantageous. Desiccants rapidly and strongly bind water, often reacting chemically with it. This strong binding makes reversibly desorbing the water from the desiccant very difficult. The third method by which to absorb water from a gas sample involves the use of molecular sieves of other ziolites.

Manning, Heidi L. K.↗

NASA NTRS1971

A Description of the Philips SO2 Monitor

Strict standards for ambient sulfur dioxide requirements in the San Francisco Bay Area result in strict criteria for monitor operations by private industry. Of nine different monitors tested, three are acceptable. One, the Phillips PW 9700, senses sulfur dioxide by coulometric reaction with bromine in a potassium bromide solution. The monitor has a high degree of sensitivity, rapid response, and stable attendance or maintenance is aided by quality construction, internal reagent supply, and elimination of reagent pump. Options include automatic zeroing and calibration, probe filter and heater, and telemetering output.

Potter, L. B.↗

NASA NTRS2000

Treatability Study of Pentaborane(9)

Procedures for the safe destruction of liquid pentaborane(9), B5H9, by solvolysis were investigated. The objective of the study was to establish the optimum conditions for a pilot plant operation that would use water, or alcohol, or water-alcohol mixtures as the solvolysis reagent. Small amounts of B5H9 sprayed from a syringe will not necessarily enflame, nor will a small pool on a spot plate. Therefore, a procedure was developed to reproducibly demonstrate the flammability of B5H9. In these tests every sample of neat B5H9 ignited and burned with a very sooty flame till the sample was consumed. The spontaneous self-ignition of B5H9 was quenched by the addition of small concentrations of ethers THF (tetrahydrofuran) or DME (1,2-dimethoxy ethane). It was found that ten percent (volume) of either provided total quenching with a large margin of safety. When these stabilized solutions were exposed to air, they decomposed and evaporated leaving a residue that was identified by nuclear magnetic resonance (NMR) analysis as boric acid. Most of the laboratory solvolysis experiments used the 90 percent B5H9, 10 percent THF solution. This mixture was safer to handle and its solvolysis reactivity was virtually identical to that of 100 percent B5H9. Reaction rates were analyzed by measurement of hydrogen evolved during the solvolysis reactions. In terms of the minimum overall complete reaction time, the data indicate that 50/50 alcohol/water is the optimum solvolysis reagent. This reaction produced a mixture of boric acid, B(OH)3, and triethoxyborane, B(OEt)3[Et = C2H5], and mixed exchange derivatives thereof.

McDonald, Joseph K.↗