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Extraterrestrial Molecular Indicators of Life Investigation (EMILI)

Future missions to Enceladus, Europa, Mars, and beyond may seek the molecular signs of extraterrestrial life through chemical analysis of acquired samples. Particularly on ocean worlds such as Enceladus and Europa, samples may contain trace ocean-borne molecular biosignatures of extant life that may or may not share similarities to those of terrestrial life. In situ analyses must be prepared to detect and characterize a wide range of possible molecular species, structures, and patterns, typically with exquisite sensitivity and within a complex, poorly-characterized planetary environment. The Extraterrestrial Molecular Indicators of Life Investigation (EMILI) is designed to meet or exceed the requirements of such missions for organic molecular analysis through a powerful combination of dual chemical separation and both optical and mass spectrometry detection techniques, realized in an integrated, compact instrument package fully compatible with anticipated flight resources and conditions. The full EMILI instrument combines two sample analysis subsystems to provide wide-ranging and complementary detection of organic compounds and inorganic salts. The Gas Analysis Processing System (GAPS) uses a chemical derivatization protocol with gas chromatography (GC) separation prior to detection in an ion trap mass spectrometer (ITMS) to enable full characterization of lower-polarity, volatile and semi-volatile molecules such as fatty acids and hydrocarbons. The Organic Capillary Electrophoresis ANalysis System (OCEANS) uses a liquid-based extraction protocol with CE separation to enable precise analysis of more water-soluble/polar compounds. OCEANS features a laser-induced fluorescence detection mode to perform ultra-sensitive quantitative analysis of chiral amino acids. In EMILI, OCEANS is additionally coupled to the same ITMS through a novel electrospray ionization interface. The common ITMS allows EMILI to identify and cross-correlate molecular species and patterns, detected through either or both protocols, of molecular weights to over 1000 u, potentially even revealing complex biosignatures such as alien oligopeptides and informational polymers.

Europa↗
NASA NTRS1997

New Fluorinated Polymers

This report summarizes progress during 1996 in our research effort along with a description of additional results associated with a TAG supplement to this grant (items 2 and 5 below). Progress is reported in five areas: 1) Polyamides Derived from [(p-HOOCC6H4)](sub 2)C(CF3)X (X= -CF3, OCH3, Cl); 2) Phosphorus-containing '12F-PEK' - Effect of Systematic Replacement of [(p-FC6H4COC6H4)](sub 2)C[(CF3)](sub 2) Monomer by [(p-FC6H4)](sub 2)(C6H5)PO; 3) Poly(ether ketone)s Derived from [(p-FC6H4COC6H4)](sub 2)(C6H5)PO; 4) New CF3-containing Organosilane Monomers and; 5) New Monomers for 12F-PEK Analogues with Improved Processability and Solubility.

Fitch, John W., III↗
NASA NTRS1991

Polyimides containing pendent siloxane groups

The incorporation of siloxane units into the backbone of aromatic polyimides has been shown to impart certain advantages over the unmodified polyimides. These include enhanced solubility, lower moisture adsorption, lower dielectric constant, improved toughness and surface modification. Also, when exposed to an atomic oxygen environment these materials form an in-situ silicate (SiO2) surface coating which protects the underlying material from further erosion. These unique advantages make polyimide-siloxanes useful in a variety of electronic and aerospace applications. As part of an effort on high performance polymeric materials for potential aerospace applications, polyimides containing pendent siloxane groups are under study. These materials were prepared by reacting a functionalized siloxane compound with polyimides containing benzhydrol groups. Thin films of the polymers exhibited glass transition temperatures ranging from 167 to 235 C. Tensile strengths and moduli measured at 23 C ranged from 11 to 14 ksi and 250 to 450 ksi, respectively. The dielectric constant was lowered substantially from that of the unmodified polyimide.

Connell, John W.↗
NASA NTRS2005

Chemical colloids versus biological colloids: a comparative study for the elucidation of the mechanism of protein fiber formation

Fiber formation from murine serum amyloid A1 (SAA) was compared to the linear aggregation and fiber formation of colloidal gold particles. Here we report the similarities of these processes. Upon incubation with acetic acid, SAA misfolds and adopts a new conformation, which we termed saa. saa apparently is less soluble than SAA in aqueous solution; it aggregates and forms nucleation units and then fibers. The fibers appear as a string of the nucleation units. Additionally, an external electric field promotes saa fiber formation. These properties of saa are reminiscent of colloidal gold formation from gold ions and one-dimensional aggregation of the gold colloids. Colloidal gold particles were also found to be capable of aggregating one-dimensionally under an electric field or in the presence of polylysine. These gold fibers resembled in structure that of saa fibers. In summary, protein aggregation and formation of fibers appear to follow the generalized principles derived in colloidal science for the aggregation of atoms and molecules, including polymers such as polypeptides. The analysis of colloidal gold formation and of one-dimensional aggregation provides a simple model system for the elucidation of some aspects of protein fiber formation.

Colloids↗
NASA NTRS2005

A Preliminary Investigation of the E-Beam Induced Polymerization of Maleimide and Norbornene End-capped Polyimides

A research area of high activity in connection with aerospace engineering has been the development of polymer thermosetting resins that can resist temperature as high as 300 C while maintaining adequate toughness, and providing ease of processing to enable low temperature and low cost composite fabrication methods. In order to meet such requirements, sequential interpenetrating polymer networks (IPNs) based on bismaleimide (BMI) and cyanate ester (CE) monomers were investigated. In these systems, a polycyanurate network is first formed in the presence of BMI and appropriate reactive diluent monomers and in a second step, a network based on the BMI is created in the presence of a fully formed polycyanurate network. The materials developed can be processed at relatively low temperature (less than 150 C) and with the aid of electron beam (EB) curing. Of major importance to the success of this work was the identification of a reactive diluent that improves ease of processing and has tailored reactivity to allow for the controlled synthesis of CE-BMI sequential IPNs. Based on solubility and reactivity of a number of reactive diluents, N-acryloylmorpholine (AMP) was selected as a comonomer for BMI copolymerization. A donor-acceptoreaction mechanism was suggested to explain the relative reactivity of a variety of reactive diluents towards maleimide functionality. The optimum processing parameters for the formation of the first network were determined through the study of metal catalyzed cure and hydrolysis of cyanate esters, whereas the reaction behavior for second network formation in terms of the influence of EB dose rate and temperature was elucidated through an in-situ kinetics study of maleimide and AMP copolymerization. Structure-property relationships were developed which allowed for the design of improved resin systems. In particular, appropriate network coupler possessing cyanate ester and maleimide functionality was synthesized to link the polycyanurate first network to the BMI/AMP second network and thus form linked sequential IPNs (LIPNs). Consequently, Tg as high as 370 C was achieved and a fracture toughness of 120 Joules per square meters was obtained for resin systems that possess adequately low viscosity for processing using liquid molding techniques at low temperature.

Palmese, Giuseppe R.↗
NASA NTRS1994

In-situ polymerized PLOT columns III: divinylbenzene copolymers and dimethacrylate homopolymers

Studies of divinylbenzene copolymers and dimethacrylate homopolymers indicate that the polymer pore size controls the separation of water and ammonia on porous-layer-open-tubular (PLOT) columns. To a lesser degree, the polarity of the polymers also affects the separation of a water-ammonia gas mixture. Our results demonstrate that the pore size can be regulated by controlling the cross-linking density or the chain length between the cross-linking functional groups. An optimum pore size will provide the best separation of water and ammonia.

NASA Discipline Exobiology↗
NASA NTRS1997

Dimerization in Highly Concentrated Solutions of Phosphoimidazolide Activated Mononucleotides

Phosphoimidazolide activated ribomononucleotides (*pN) are useful substrates for the non-enzymatic synthesis of polynucleotides. However, dilute neutral aqueous solutions of *pN typically yield small amounts of dimers and traces of polymers; most of *pN hydrolyzes to yield nucleoside 5'-monophosphate. Here we report the self-condensation of nucleoside 5'-phosphate 2- methylimidazolide (2-MeImpN with N = cytidine, uridine or guanosine) in the presence of Mg2(+) in concentrated solutions, such as might have been found in an evaporating lagoon on prebiotic Earth. The product distribution indicates that oligomerization is favored at the expense of hydrolysis. At 1.0 M, 2-MelmpU and 2-MelmpC produce about 65% of oligomers including 4% of the 3',5'-Iinked dimer. Examination of the product distribution of the three isomeric dimers in a self-condensation allows identification of reaction pathways that lead to dimer formation. Condensations in a concentrated mixture of all three nucleotides (U,C,G mixtures) is made possible by the enhanced solubility of 2-MeImpG in such mixtures. Although percent yield of intemucleotide linked dimers is enhanced as a function of initial monomer concentration, pyrophosphate dimer yields remain practically unchanged at about 20% for 2-MelmpU, 16% for 2-MeImpC and 25% of the total pyrophosphate in the U,C,G mixtures. The efficiency by which oligomers are produced in these concentrated solutions makes the evaporating lagoon scenario a potentially interesting medium for the prebiotic synthesis of dimers and short RNAs.

Kanavarioti, Anastassia↗
NASA NTRS2018

Enantiomer Excesses in Meteoritic Organic Compounds: a Role for Radiation-Magnetism?

Carbonaceous chondrites contain an insoluble “macromolecular” carbon phase as well as discrete soluble organic compounds including amino acids and sugar derivatives. Both the macromolecular carbon and the sugar derivatives are thought to have formed through aqueous formaldehyde chemistry. Formaldehyde is a ubiquitous molecule in interstellar space environments and therefore its chemistry was likely important during the formation of the Earth and other planets. It was also likely delivered throughout Earth's history: it is found in comets and (asteroidal) meteorites. Among the reactions of formaldehyde, those in water are thought to be an important part of the primordial route to today’s nucleic acids, DNA and RNA. A plausible pre-biotic path to these biopolymers would begin with the "formose" reaction, the self-reaction of formaldehyde in an alkaline aqueous medium. Formaldehyde's inclusion in the young solar system’s planets would have provided a relatively fast route to a variety of hydroxylated compounds related to nucleic acids and metabolism, including sugars, sugar acids, sugar alcohols, and formaldehyde polymers.

Cooper, G.↗
NASA NTRS2004

Improved Thermoplastic/Iron-Particle Transformer Cores

A method of fabricating improved transformer cores from composites of thermoplastic matrices and iron-particles has been invented. Relative to commercially available laminated-iron-alloy transformer cores, the cores fabricated by this method weigh less and are less expensive. Relative to prior polymer-matrix/ iron-particle composite-material transformer cores, the cores fabricated by this method can be made mechanically stronger and more magnetically permeable. In addition, whereas some prior cores have exhibited significant eddy-current losses, the cores fabricated by this method exhibit very small eddy-current losses. The cores made by this method can be expected to be attractive for use in diverse applications, including high-signal-to-noise transformers, stepping motors, and high-frequency ignition coils. The present method is a product of an experimental study of the relationships among fabrication conditions, final densities of iron particles, and mechanical and electromagnetic properties of fabricated cores. Among the fabrication conditions investigated were molding pressures (83, 104, and 131 MPa), and molding temperatures (250, 300, and 350 C). Each block of core material was made by uniaxial-compression molding, at the applicable pressure/temperature combination, of a mixture of 2 weight percent of LaRC (or equivalent high-temperature soluble thermoplastic adhesive) with 98 weight percent of approximately spherical iron particles having diameters in the micron range. Each molded block was cut into square cross-section rods that were used as core specimens in mechanical and electromagnetic tests. Some of the core specimens were annealed at 900 C and cooled slowly before testing. For comparison, a low-carbon-steel core was also tested. The results of the tests showed that density, hardness, and rupture strength generally increased with molding pressure and temperature, though the correlation was rather weak. The weakness of the correlation was attributed to the pores in the specimens. The maximum relative permeabilities of cores made without annealing ranged from 30 to 110, while those of cores made with annealing ranged from 900 to 1,400. However, the greater permeabilities of the annealed specimens were not associated with noticeably greater densities. The major practical result of the investigation was the discovery of an optimum distribution of iron-particle sizes: It was found that eddy-current losses in the molded cores were minimized by using 100 mesh (corresponding to particles with diameters less than or equal to 100 m) iron particles. The effect of optimization of particle sizes on eddy-current losses is depicted in the figure.

Wincheski, Russell A.↗
NASA NTRS2017

Sample Processor for Life on Icy Worlds (SPLIce): Design and Test Results

We report the design, development, and testing of the Sample Processor for Life on Icy Worlds (SPLIce) system, a microfluidic sample processor to enable autonomous detection of signatures of life and measurements of habitability parameters in Ocean Worlds. This monolithic fluid processing-and-handling system (Figure 1; mass 0.5 kg) retrieves a 50-L-volume sample and prepares it to supply a suite of detection instruments, each with unique preparation needs. SPLIce has potential applications in orbiter missions that sample ocean plumes, such as found in Saturns icy moon Enceladus, or landed missions on the surface of icy satellites, such as Jupiters moon Europa. Answering the question Are we alone in the universe? is captivating and exceptionally challenging. Even general criteria that define life very broadly include a significant role for water [1,2]. Searches for extinct or extant life therefore prioritize locations of abundant water whether in ancient (Mars), or present (Europa and Enceladus) times. Only two previous planetary missions had onboard fluid processing: the Viking Biology Experiments [3] and Phoenixs Wet Chemistry Laboratory (WCL) [4]. SPLIce differs crucially from those systems, including its capability to process and distribute L-volume samples and the integration autonomous control of a wide range of fluidic functions, including: 1) retrieval of fluid samples from an evacuated sample chamber; 2) onboard multi-year storage of dehydrated reagents; 3) integrated pressure, pH, and conductivity measurement; 4) filtration and retention of insoluble particles for microscopy; 5) dilution or vacuum-driven concentration of samples to accommodate instrument working ranges; 6) removal of gas bubbles from sample aliquots; 7) unidirectional flow (check valves); 8) active flow-path selection (solenoid-actuated valves); 9) metered pumping in 100 nL volume increments. The SPLIce manifold, made of three thermally fused layers of precision-machined cyclo-olefin polymer, supports all fluidic components (Figure 1) and integrated microchannels (125 x 250 m). Fluid is pumped by a stepper-motor-driven pump (Lee Co.). The functionality of the integrated MEMS pressure sensor (Honeywell) and passive check valves (Figure 2) were tested in conjunction with our newly designed integral bubble traps (Figure 3) and hydrophobic membrane-based concentrator (Figure 4). The concentrator (initially tested as a standalone component) demonstrated 5-fold vacuum-evaporative concentration. Polyethylene fused bead beds (PEFBBs; 50 porosity) store drylyophilized buffers, calibrants, and fluorescent dyes, and also promote mixing of sample with calibrant, dye, or H2O. Software-controlled automated tests demonstrated successful 1) fluid delivery to each component 2) valve and pump synchronization 3) sample aliquot delivery to instrument interface ports, and 4) rehydration of vacuum-dried fluorescent dye. In Figure 5, fluorescein on PEFBBs was rehydrated for 15 min using a pump-delivered water aliquot; it is displaced as H2O enters the bottom of the channel and pushes the dye into a check valve. Ultimately, SPLIce will fluorescently label amino acids in the sample for microchip-based electrophoretic (MCE) chiral separation and detection to seek and quantify key organic bio-signatures [5]; it will also deliver sample to a microfluidic version of WCL (mWCL) to measure soluble ions and redox-active species.

Life detection↗
NASA NTRS2001

Safer Aviation Materials Tested

A series of thermally stable polymer samples were tested. These materials are called low heat release materials and are designed for aircraft interior decorative materials. The materials are designed to give off a minimum amount of noxious gases when heated, which increases the possibility that people can escape from a burning aircraft. New cabin materials have suitably low heat release so that fire does not spread, toxic chemicals are not given off, and the fire-emergency escape time for crew and passengers is lengthened. These low heat-release materials have a variety of advantages and applications: interiors for ground-based facilities, interiors of space vehicles, and many commercial fire-protection environments. A microscale combustion calorimeter at the Federal Aviation Administration's (FAA) Technical Center tested NASA Langley Research Center materials samples. The calorimeter is shown. A sharp, quantitative, and reproducible heat-release-rate peak is obtained in the microscale heat-release-rate test. The newly tested NASA materials significantly reduced the heat release capacity and total heat release. The thermal stability and flammability behavior of the samples was very good. The new materials demonstrated a factor of 4 reduction in total heat release over ULTEM (a currently used material). This information is provided in the following barchart. In other tests, the materials showed greater than a factor 9 reduction in heat-release capacity over ULTEM. The newly tested materials were developed for low dielectric constant, low color, and good solubility. A scale up of the material samples is needed to determine the repeatability of the performance in larger samples. Larger panels composed of the best candidate materials will be tested in a larger scale FAA Technical Center fire facility. The NASA Glenn Research Center, Langley (Jeff Hinkley), and the FAA Technical Center (Richard Lyon) cooperatively tested these materials for the Accident Mitigation aspects of Fire Prevention under NASA's Aviation Safety Program.

Palaszewski, Bryan A.↗
NASA NTRS2004

Did the Pre-RNA World Rest Upon DNA Molecules?

The isolation of a DNA sequence that catalyzes the ligation of oligodeoxynucleotides via the formation of 3' - 5' phosphodiester linkage significance in selection experiments has been reported. Ball recently used this to discuss the possibility that natural DNA molecules may have formed in the primitive Earth leading to the origin of life. As noted by Ferris and Usher, if metabolic pathways evolved backwards, it could be argued that the biosynthesis of 2-deoxyribose from ribose suggests that RNA came from DNA. As summarized elsewhere, there are several properties of deoxyribose which could be interpreted to support the possibility that DNA-like molecules arose prior to the RNA world. For example, 2-deoxyribose is slightly more soluble than ribose (which may have been an advantage in a drying pool scenario), may have been more reactive under possible prebiotic conditions (it forms a nucleoside approx. 150 times faster than ribose with the alternative base urazole at 25 C), while it decomposes in solution (approximately 2.6 times more slowly than ribose at 100 C). Other advantages of DNA over RNA are that it has one fewer chiral center, has a greater stability at the 8.2 pH value of the current oceans, and does not has the 2'5' and 3'5' ambiguity in polymerizations. Yet, there is strong molecular biological and biochemical evidence that RNA was featured in the biology well before the last common ancestor. The presence of sugar acids, including both ribo- and deoxysugar acids, in the 4.6 Ga old Murchison meteorite suggest that both may have been available in the primitive Earth, derived from the accretion of extraterrestrial sources and/or from endogenous processes involving formaldehyde and its derivatives. However, the abiotic synthesis of deoxyribose, ribose, and other sugars from glyceraldehyde and acetaldehyde under alkaline conditions is inefficient and unespecific. Although sugars are labile compounds, the role of cyanamide or borate minerals in the stabilization of the cyclic forms of ribose and other pentoses has recently been demonstrated. Nonetheless, the assumption either RNA or DNA was the first genetic material needs to be supplemented by laboratory models demonstrating that the prebiotic synthesis of activated beta-D-(deoxy)ribonucleotides and their polymers was feasible. As of today such evidence is lacking, and there is no convincing synthesis of any nucleotide, since all model experiments produce complex mixtures of products in which there is no preferential synthesis of chiral D-nucleotides. This strongly suggests that both DNA and RNA may have been preceded by pairing structures much simpler than extant nucleic acids. It is doubtful that DNA molecules, or indeed other (de0xy)ribofuranoid oligonucleotides formed the basis of these as yet undescribed pre-RNA worlds.

Lazcano, Antonio↗
NASA NTRS2003

Self-Propagating Frontal Polymerization in Water at Ambient Pressure

Advances in polymer chemistry have led to the development of monomers and initiation agents that enable propagating free-radical polymerization fronts to exist. These fronts are driven by the exothermicity of the polymerization reaction and the transport of heat from the polymerized product to the reactant monomer/solvent/initiator solution. The thermal energy transported to the reactant solution causes the initiator to decompose, yielding free radicals, which start the free radical polymerization process as discussed in recent reviews. The use of polymerization processes based on propagating fronts has numerous applications. Perhaps the most important of these is that it enables rapid curing of polymers without external heating since the polymerization process itself provides the high temperatures necessary to initiate and sustain polymerization. This process also enables more uniform curing of arbitrarily thick samples since it does not rely on heat transfer from an external source, which will necessarily cause the temperature history of the sample to vary with distance from the surface according to a diffusion-like process. Frontal polymerization also enables filling and sealing of structures having cavities of arbitrary shape without having to externally heat the structure. Water at atmospheric pressure is most convenient solvent to employ and the most important for practical applications (because of the cost and environmental issues associated with DMSO and other solvents). Nevertheless, to our knowledge, steady, self-propagating polymerization fronts have not been reported in water at atmospheric pressure. Currently, polymerization fronts require a high boiling point solvent (either water at high pressures or an alternative solvent such as dimethyl sulfoxide (DMSO) (boiling point 189 C at atmospheric pressure.) Early work on frontal polymerization, employed pressures up to 5000 atm in order to avoid boiling of the monomer/solvent/initiator solution. High boiling point solutions are needed because in order to produce a propagating front, a high front temperature is needed to produce sufficiently rapid decomposition of the free radical initiator and subsequent free radical polymerization and heat release at a rate faster than heat losses remove thermal energy from the system. (While the conduction heat loss rate increases linearly with temperature, the free radical initiator decomposition is a high activation energy process whose rate increases much more rapidly than linearly with temperature, thus as the temperature decreases, the ratio of heat loss to heat generation increases, eventually leading to extinction of the front if the temperature is too low.) In order to obtain atmospheric pressure frontal polymerization in water, it is necessary to identify a monomer/initiator combination that is water soluble and will not extinguish even when the peak temperature (T*) is less than 100 C. In this work acrylic acid (AA) was chosen as the monomer because is it one of the most reactive monomers and can polymerize readily at low temperatures even without initiators. Ammonium persulfate (AP) was chosen as the initiator because it decomposes readily at low temperatures, produces relatively few bubbles and is commercially available. The propagation rates and extinction conditions of the fronts are studied for a range of AA and AP concentrations. Small amounts of fumed silica powder (Cab-o-sil, Cabot Corporation) were added to the solutions to inhibit buoyancy induced convection in the solutions; future studies will investigate the effects of buoyant convection within the solutions.

Olten, Nesrin↗