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NASA NTRS2002

Nanoscale and Microscale Iron Emulsions for Treating DNAPL

This study demonstrated the feasibility of using emulsified nanoscale and microscale iron particles to enhance dehalogenation of (Dense Non-Aqueous Phase Liquid) DNAPL free-phase. The emulsified system consisted of a surfactant-stabilized, biodegradable oil-in-water emulsion with nanoscale or microscale iron particles contained within the emulsion droplets. It was demonstrated that DNAPLs, such as trichloroethene (TCE), diffuse through the oil membrane of the emulsion particle whereupon they reach an aqueous interior and the surface of an iron particle where dehalogenation takes place. The hydrocarbon reaction by-products of the dehalogenation reaction, primarily ethene (no chlorinated products detected), diffuse out of the emulsion droplet. This study also demonstrated that an iron-emulsion system could be delivered in-situ to the DNAPL pool in a soil matrix by using a simulated push well technique. Iron emulsions degraded pure TCE at a rate comparable to the degradation of dissolved phase TCE by iron particles, while pure iron had a very low degradation rate for free-phase TCE. The iron-emulsion systems can be injected into a sand matrix where they become immobilized and are not moved by flowing water. It has been documented that surfactant micelles possess the ability to pull pooled TCE into emulsion droplets where degradation of TCE takes place.

Geiger, Cherie L.↗

NASA NTRS2003

Zero-Valent Metal Emulsion for Reductive Dehalogenation of DNAPLS

A zero-valent metal emulsion is used to dehalogenate solvents, such as pooled dense non-aqueous phase liquids (DNAPLs), including trichloroethylene (TCE). The zero-valent metal emulsion contains zero-valent metal particles, a surfactant, oil and water. The preferred zero-valent metal particles are nanoscale and microscale zero-valent iron particles

Debra R Reinhart↗

NASA NTRS2003

Infrared Spectroscopy as a Chemical Fingerprinting Tool

Infrared (IR) spectroscopy is a powerful analytical tool in the chemical fingerprinting of materials. Any sample material that will interact with infrared light produces a spectrum and, although normally associated with organic materials, inorganic compounds may also be infrared active. The technique is rapid, reproducible and usually non-invasive to the sample. That it is non-invasive allows for additional characterization of the original material using other analytical techniques including thermal analysis and RAMAN spectroscopic techniques. With the appropriate accessories, the technique can be used to examine samples in liquid, solid or gas phase. Both aqueous and non-aqueous free-flowing solutions can be analyzed, as can viscous liquids such as heavy oils and greases. Solid samples of varying sizes and shapes may also be examined and with the addition of microscopic IR (microspectroscopy) capabilities, minute materials such as single fibers and threads may be analyzed. With the addition of appropriate software, microspectroscopy can be used for automated discrete point or compositional surface area mapping, with the latter providing a means to record changes in the chemical composition of a material surface over a defined area. Due to the ability to characterize gaseous samples, IR spectroscopy can also be coupled with thermal processes such as thermogravimetric (TG) analyses to provide both thermal and chemical data in a single run. In this configuration, solids (or liquids) heated in a TG analyzer undergo decomposition, with the evolving gases directed into the IR spectrometer. Thus, information is provided on the thermal properties of a material and the order in which its chemical constituents are broken down during incremental heating. Specific examples of these varied applications will be cited, with data interpretation and method limitations further discussed.

Huff, Timothy L.↗

NASA NTRS1997

Redox chemistry at liquid/liquid interfaces

The interface between two immiscible liquids with immobilized photosynthetic pigments can serve as the simplest model of a biological membrane convenient for the investigation of photoprocesses accompanied by spatial separation of charges. As it follows from thermodynamics, if the resolvation energies of substrates and products are very different, the interface between two immiscible liquids may act as a catalyst. Theoretical aspects of charge transfer reactions at oil/water interfaces are discussed. Conditions under which the free energy of activation of the interfacial reaction of electron transfer decreases are established. The activation energy of electron transfer depends on the charges of the reactants and dielectric permittivity of the non-aqueous phase. This can be useful when choosing a pair of immiscible solvents to decrease the activation energy of the reaction in question or to inhibit an undesired process. Experimental interfacial catalytic systems are discussed. Amphiphilic molecules such as chlorophyll or porphyrins were studied as catalysts of electron transfer reactions at the oil/water interface.

Non-NASA Center↗

NASA NTRS2003

In Situ Remediation of Polychlorinated Bephenyls Using Palladium Coated Iron or Magnesium

The remediation of polychlorinated biphenyls (PCBs) and other chlorinated synthetic aromatic compounds are of great concern due to their toxicity and persistence in the environment. When released into the environment, PCBs are sorbed to particulate matter that can then disperse over large areas. Although the US Environmental Protection Agency (EPA) has banned the manufacture of PCBs since 1979, they are still present in the environment posing possible adverse health affects to both humans and animals. Thus, it is of utmost importance to develop a method that remediates PCB-contaminated soil, sediments, and water. The objective of our research was to develop an in-situ PCB remediation technique that is applicable for the treatment of soils and sediments. Previous research conducted at the University of Central Florida (UCF) proved the feasibility of using an emulsified system to dehalogenate a dense non-aqueous phase liquid (DNAPL) source, such as TCE, in the subsurface by means of an in-situ injection. The generation of a hydrophobic emulsion system drew the DNAPL TCE, through the oil membrane where it diffused to the iron particle and underwent degradation. TCE continued to enter, diffuse, degrade and exit the droplet maintaining a concentration gradient across the membrane, thus maintaining the driving force of the reaction.

Geiger, Cherie L.↗

NASA NTRS2004

Ionic Liquids and New Proton Exchange Membranes for Fuel Cells

There is currently a great surge of activity in fuel cell research as laboratories across the world seek to take advantage of the high energy capacity provided by &el cells relative to those of other portable electrochemical power systems. Much of this activity is aimed at high temperature fie1 cells, and a vital component of such &el cells must be the availability of a high temperature stable proton-permeable membrane. NASA Glenn Research Center is greatly involved in developing this technology. Other approaches to the high temperature fuel cell involve the use of single- component or almost-single-component electrolytes that provide a path for protons through the cell. A heavily researched case is the phosphoric acid fuel cell, in which the electrolyte is almost pure phosphoric acid and the cathode reaction produces water directly. The phosphoric acid fie1 cell delivers an open circuit voltage of 0.9 V falling to about 0.7 V under operating conditions at 170 C. The proton transport mechanism is mainly vehicular in character according to the viscosity/conductance relation. Here we describe some Proton Transfer Ionic Liquids (PTILs) with low vapor pressure and high temperature stability that have conductivities of unprecedented magnitude for non-aqueous systems. The first requirement of an ionic liquid is that, contrary to experience with most liquids consisting of ions, it must have a melting point that is not much above room temperature. The limit commonly suggested is 100 C. PTILs constitute an interesting class of non-corrosive proton-exchange electrolyte, which can serve well in high temperature (T = 100 - 250 C) fuel cell applications. We will present cell performance data showing that the open circuit voltage output, and the performance of a simple H2(g)Pt/PTIL/Pt/O2(g) fuel cell may be superior to those of the equivalent phosphoric acid electrolyte fuel cell both at ambient temperature and temperatures up to and above 200 C. My work at NASA Glenn Research Center during this summer is to develop and characterize proton exchange membranes doped with ionic liquids. The main techniques used to characterize these materials are: Impedance Spectroscopy, NMR, DSC, TGA, DMA, IR, and SEM ...

Belieres, Jean-Philippe↗

NASA NTRS2006

Zero-Valent Metal Emulsion for Reductive Dehalogenation of DNAPLs

A zero-valent metal emulsion is used to dehalogenate solvents, such as pooled dense non-aqueous phase liquids (DNAPLs), including trichloroethylene (TCE). The zero-valent metal emulsion contains zero-valent metal particles, a surfactant, oil and water, The preferred zero-valent metal particles are nanoscale and microscale zero-valent iron particles.

Reinhart, Debra R.↗

NASA NTRS2005

Valiant 'Zero-Valent' Effort Restores Contaminated Grounds

Dense non-aqueous phase liquids (DNAPLs) are chemical compounds that can contaminate soil and groundwater to the point of irreparability. These substances are only slightly soluble in water, and are much denser than water. Because of their solubility, DNAPLs form separate liquid phases in groundwater, and because of their density, DNAPLs sink in aquifers instead of floating at the water table, making it extremely difficult to detect their presence. If left untreated in the ground, they can taint fresh water sources. Common DNAPLs include chlorinated hydrocarbon compounds such as carbon tetrachloride, chloroform, tetrachloroethylene, and trichloroethylene. Trichloroethylene was used during the early days of the Space Program, as a solvent for flushing rocket engines, and for metal cleaning and degreasing of equipment, electronics, and heavy machinery. As a result, areas of Cape Canaveral s Launch Complex 34, the site of several historic Saturn rocket launches occurring from 1959 to 1968, were polluted with chlorinated DNAPLs. Through the direction and guidance of Dr. Jacqueline Quinn, an environmental engineer in the Spaceport Engineering and Technology Directorate at NASA s Kennedy Space Center, a biodegradable environmental cleanup technology was developed to reductively dechlorinate DNAPL sources in polluted water at Launch Complex 34. It was important for Kennedy to nip this problem in the bud, in light of the fact that the Space Center is also a National Wildlife Refuge, home to thousands of shorebirds, endangered sea turtles and eagles, manatees, alligators, and diverse habitats that include brackish marshes and salt water estuaries. The success in remediating this historic launch site has led to numerous commercial applications that are restoring the health of our environmental surroundings.

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NASA NTRS2008

Low-Temperature Supercapacitors

An effort to extend the low-temperature operational limit of supercapacitors is currently underway. At present, commercially available non-aqueous supercapacitors are rated for a minimum operating temperature of -40 C. A capability to operate at lower temperatures would be desirable for delivering power to systems that must operate in outer space or in the Polar Regions on Earth. Supercapacitors (also known as double-layer or electrochemical capacitors) offer a high power density (>1,000 W/kg) and moderate energy density (about 5 to 10 Wh/kg) technology for storing energy and delivering power. This combination of properties enables delivery of large currents for pulsed applications, or alternatively, smaller currents for low duty cycle applications. The mechanism of storage of electric charge in a supercapacitor -- at the electrical double-layer formed at a solid-electrode/liquid-electrolyte interface -- differs from that of a primary or secondary electrochemical cell (i.e., a battery) in such a manner as to impart a long cycle life (typically >10(exp 6) charge/discharge cycles).

Brandon, Erik J.↗

NASA NTRS2008

Increasing Discharge Capacities of Li-(CF)(sub n) Cells

An electrolyte additive has shown promise as a means of increasing the sustainable rates of discharge and, hence, the discharge capacities, of lithiumpoly(carbon monofluoride) electrochemical power cells. Lithium-poly(carbon monofluoride) [Li-(CF)n] cells and batteries offer very high specific energies practical values of about 600 W.h/g and a theoretical maximum value of 2,180 W.h/kg. However, because Li-(CF)n cells and batteries cannot withstand discharge at high rates, they have been relegated to niche applications that involve very low discharge currents over times of the order of hundreds to thousands of hours. Increasing the discharge capacities of Li- (CF)n batteries while maintaining high practical levels of specific energy would open new applications for these batteries. During the discharge of a Li-(CF)n cell, one of the electrochemical reactions causes LiF to precipitate at the cathode. LiF is almost completely insoluble in most non-aqueous solvents, including those used in the electrolyte solutions of Li-(CF)n cells. LiF is electrochemically inactive and can block the desired transport of ions at the cathode, and, hence, the precipitation of LiF can form an ever-thickening film on the cathode that limits the rate of discharge.

Whitacre, Jay↗

NASA NTRS2009

Li/CFx Cells Optimized for Low-Temperature Operation

Some developments reported in prior NASA Tech Briefs articles on primary electrochemical power cells containing lithium anodes and fluorinated carbonaceous (CFx) cathodes have been combined to yield a product line of cells optimized for relatively-high-current operation at low temperatures at which commercial lithium-based cells become useless. These developments have involved modifications of the chemistry of commercial Li/CFx cells and batteries, which are not suitable for high-current and low-temperature applications because they are current-limited and their maximum discharge rates decrease with decreasing temperature. One of two developments that constitute the present combination is, itself, a combination of developments: (1) the use of sub-fluorinated carbonaceous (CFx wherein x<1) cathode material, (2) making the cathodes thinner than in most commercial units, and (3) using non-aqueous electrolytes formulated especially to enhance low-temperature performance. This combination of developments was described in more detail in High-Energy-Density, Low- Temperature Li/CFx Primary Cells (NPO-43219), NASA Tech Briefs, Vol. 31, No. 7 (July 2007), page 43. The other development included in the present combination is the use of an anion receptor as an electrolyte additive, as described in the immediately preceding article, "Additive for Low-Temperature Operation of Li-(CF)n Cells" (NPO- 43579). A typical cell according to the present combination of developments contains an anion-receptor additive solvated in an electrolyte that comprises LiBF4 dissolved at a concentration of 0.5 M in a mixture of four volume parts of 1,2 dimethoxyethane with one volume part of propylene carbonate. The proportion, x, of fluorine in the cathode in such a cell lies between 0.5 and 0.9. The best of such cells fabricated to date have exhibited discharge capacities as large as 0.6 A h per gram at a temperature of 50 C when discharged at a rate of C/5 (where C is the magnitude of the current, integrated for one hour, that would amount to the nominal charge capacity of a cell).

Smart, Marshall C.↗

NASA NTRS2007

Lithium Dinitramide as an Additive in Lithium Power Cells

Lithium dinitramide, LiN(NO2)2 has shown promise as an additive to nonaqueous electrolytes in rechargeable and non-rechargeable lithium-ion-based electrochemical power cells. Such non-aqueous electrolytes consist of lithium salts dissolved in mixtures of organic ethers, esters, carbonates, or acetals. The benefits of adding lithium dinitramide (which is also a lithium salt) include lower irreversible loss of capacity on the first charge/discharge cycle, higher cycle life, lower self-discharge, greater flexibility in selection of electrolyte solvents, and greater charge capacity. The need for a suitable electrolyte additive arises as follows: The metallic lithium in the anode of a lithium-ion-based power cell is so highly reactive that in addition to the desired main electrochemical reaction, it engages in side reactions that cause formation of resistive films and dendrites, which degrade performance as quantified in terms of charge capacity, cycle life, shelf life, first-cycle irreversible capacity loss, specific power, and specific energy. The incidence of side reactions can be reduced through the formation of a solid-electrolyte interface (SEI) a thin film that prevents direct contact between the lithium anode material and the electrolyte. Ideally, an SEI should chemically protect the anode and the electrolyte from each other while exhibiting high conductivity for lithium ions and little or no conductivity for electrons. A suitable additive can act as an SEI promoter. Heretofore, most SEI promotion was thought to derive from organic molecules in electrolyte solutions. In contrast, lithium dinitramide is inorganic. Dinitramide compounds are known as oxidizers in rocket-fuel chemistry and until now, were not known as SEI promoters in battery chemistry. Although the exact reason for the improvement afforded by the addition of lithium dinitramide is not clear, it has been hypothesized that lithium dinitramide competes with other electrolyte constituents to react with lithium on the surface of the anode to form a beneficial SEI. Apparently, nitrides and oxides that result from reduction of lithium dinitramide on the anode produce a thin, robust SEI different from the SEIs formed from organic SEI promoters. The SEI formed from lithium dinitramide is more electronically insulating than is the film formed in the presence of an otherwise identical electrolyte that does not include lithium dinitramide. SEI promotion with lithium dinitramide is useful in batteries with metallic lithium and lithium alloy anodes.

Gorkovenko, Alexander A.↗

NASA NTRS2010

Supercapacitor Electrolyte Solvents with Liquid Range Below -80 C

A previous NASA Tech Brief ["Low-Temperature Supercapacitors" (NPO-44386) NASA Tech Briefs, Vol. 32, No 7 (July 2008), page 32] detailed ongoing efforts to develop non-aqueous supercapacitor electrolytes capable of supporting operation at temperatures below commercially available cells (which are typically limited to charging and discharging at > or equal to -40 C). These electrolyte systems may enable energy storage and power delivery for systems operating in extreme environments, such as those encountered in the Polar regions on Earth or in the exploration of space. Supercapacitors using these electrolytes may also offer improved power delivery performance at moderately low temperatures (e.g. -40 to 0 C) relative to currently available cells, offering improved cold-cranking and cold-weather acceleration capabilities for electrical or hybrid vehicles. Supercapacitors store charge at the electrochemical double-layer, formed at the interface between a high surface area electrode material and a liquid electrolyte. The current approach to extending the low-temperature limit of the electrolyte focuses on using binary solvent systems comprising a high-dielectric-constant component (such as acetonitrile) in conjunction with a low-melting-point co-solvent (such as organic formates, esters, and ethers) to depress the freezing point of the system, while maintaining sufficient solubility of the salt. Recent efforts in this area have led to the identification of an electrolyte solvent formulation with a freezing point of -85.7 C, which is achieved by using a 1:1 by volume ratio of acetonitrile to 1,3-dioxolane

Brandon, Erik↗

NASA NTRS2010

Solutions Remediate Contaminated Groundwater

During the Apollo Program, NASA workers used chlorinated solvents to clean rocket engine components at launch sites. These solvents, known as dense non-aqueous phase liquids, had contaminated launch facilities to the point of near-irreparability. Dr. Jacqueline Quinn and Dr. Kathleen Brooks Loftin of Kennedy Space Center partnered with researchers from the University of Central Florida's chemistry and engineering programs to develop technology capable of remediating the area without great cost or further environmental damage. They called the new invention Emulsified Zero-Valent Iron (EZVI). The groundwater remediation compound is cleaning up polluted areas all around the world and is, to date, NASA's most licensed technology.

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NASA NTRS2005

Application of Emulsified Zero-Valent Iron to Marine Environments

Contamination of marine waters and sediments with heavy metals and dense non-aqueous phase liquids (DNAPLs) including chlorinated solvents, pesticides and PCBs pose ecological and human health risks through the contaminant's potential bioaccumulation in fish, shellfish and avian populations. The contaminants enter marine environments through improper disposal techniques and storm water run-off. Current remediation technologies for application to marine environments include costly dredging and off-site treatment of the contaminated media. Emulsified zero-valent iron (EZVI) has been proven to effectively degrade dissolved-phase and DNAPL-phase contaminants in freshwater environments on both the laboratory and field-scale level. However, the application to marine environments is only just being explored. This paper discusses the potential use of EZVI in brackish and saltwater environments, with supporting laboratory data detailed. Laboratory studies were performed in 2005 to establish the effectiveness of EZVI to degrade trichloroethylene (TCE) in saltwater. Headspace vials were setup to determine the kinetic rate of TCE degradation using EZVI in seawater. The reaction vials were analyzed by Gas Chromatographic/Flame Ionization Detection (GC/FID) for ethene production after a 48 day period using a GC/FID Purge and Trap system. Analytical results showed that EZVI was very effective at degrading TCE. The reaction by-products (ethene, acetylene and ethane) were produced at 71% of the rate in seawater as in the fresh water controls. Additionally, iron within the EZVI particles was protected from oxidation of the corrosive seawater, allowing EZVI to perform in an environment where zero-valent iron alone could not compete. Laboratory studies were also performed to establish the effectiveness of emulsified zero-valent metal (EZVM) to remove dissolved-phase cadmium and lead found in seawater. EZVM is comprised of a combination of magnesium and iron metal surrounded by the same oil/surfactant membrane used in EZVI. The removal of cadmium and lead from a seawater matrix is a unique challenge. It requires a system that is resistant to the corrosive nature of seawater while removing specific ions that are in a relatively low concentration compared to naturally occurring seawater salts. Laboratory studies conducted show greater than 99% removal of lead and 96% removal of cadmium from a seawater solution spiked at 5 mg/L that was treated with an Emulsified Zero-Valent Metal (EZVM). The cadmium and lead are removed from the solution as they transport across the emulsion membrane and plate out onto the zero-valent metal surface.

Brooks, Kathleen B.↗

NASA NTRS2006

Application of Emulsified Zero-Valent Iron to Marine Environments

Quinn, Jacqueline W.↗

NASA NTRS2006

Evaluating Trichloroethylene Degradation Using Differing Nano- and Micro-Scale Iron Particles

Trichioroethylene, or TCE, is a central nervous system depressant and possible carcinogen, as well as a persistent groundwater pollutant. TCE exists in the aquifer either as free product in the form of a dense non-aqueous phase liquid (DNAPL) or as a dissolved-phase constituent. It is only slightly soluble in water, so dissolution of the contaminant is a long-term process and in-situ remediation is difficult. To remedy this, NASA and the University of Central Florida developed Emulsified Zero-Valent Iron, or EZVI. The emulsion droplet contains ZVI particles and water encapsulated by an oil/surfactant membrane, and effectively penetrates to degrade DNAPL-phase TCE. To maximize the efficiency of this process, several commercially available ZVIs of radically different particle sizes and morphologies both in emulsion and as neat (unemulsified) metal were evaluated for relative effectiveness at TCE degradation.

Berger, Cristina M.↗

NASA NTRS2012

NASA Tech Briefs, November 2012

The topics include: Visual System for Browsing, Analysis, and Retrieval of Data (ViSBARD); Time-Domain Terahertz Computed Axial Tomography NDE System; Adaptive Sampling of Time Series During Remote Exploration; A Tracking Sun Photometer Without Moving Parts; Surface Temperature Data Analysis; Modular, Autonomous Command and Data Handling Software with Built-In Simulation and Test; In-Situ Wire Damage Detection System; Amplifier Module for 260-GHz Band Using Quartz Waveguide Transitions; Wideband Agile Digital Microwave Radiometer; Buckyball Nucleation of HiPco Tubes; FACT, Mega-ROSA, SOLAROSA; An Integrated, Layered-Spinel Composite Cathode for Energy Storage Applications; Engineered Multifunctional Surfaces for Fluid Handling; Polyolefin-Based Aerogels; Adjusting Permittivity by Blending Varying Ratios of SWNTs; Gravity-Assist Mechanical Simulator for Outreach; Concept for Hydrogen-Impregnated Nanofiber/Photovoltaic Cargo Stowage System; DROP: Durable Reconnaissance and Observation Platform; Developing Physiologic Models for Emergency Medical Procedures Under Microgravity; Spectroscopic Chemical Analysis Methods and Apparatus; Low Average Sidelobe Slot Array Antennas for Radiometer Applications; Motion-Corrected 3D Sonic Anemometer for Tethersondes and Other Moving Platforms; Water Treatment Systems for Long Spaceflights; Microchip Non-Aqueous Capillary Electrophoresis (MicronNACE) Method to Analyze Long-Chain Primary Amines; Low-Cost Phased Array Antenna for Sounding Rockets, Missiles, and Expendable Launch Vehicles; Mars Science Laboratory Engineering Cameras; Seismic Imager Space Telescope; Estimating Sea Surface Salinity and Wind Using Combined Passive and Active L-Band Microwave Observations; A Posteriori Study of a DNS Database Describing Super critical Binary-Species Mixing; Scalable SCPPM Decoder; QuakeSim 2.0; HURON (HUman and Robotic Optimization Network) Multi-Agent Temporal Activity Planner/Scheduler; MPST Software: MoonKommand

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