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DOE OSTI2025

Ammonia Synthesis under Ambient Conditions: Insights into Water–Nitrogen–Magnetite Interfaces

New routes for transforming nitrogen into ammonia at ambient conditions would be a milestone toward an energy efficient and economically attractive production route in comparison to the traditional Haber-Bosch process. Recently, the synthesis of ammonia from water and nitrogen at room temperature and atmospheric pressure has been reported to be catalyzed by Fe 3 O 4 at the air-water interface. By integrating ambient pressure X-ray photoelectron spectroscopy and ab initio molecular dynamics and free energy calculations, we investigate the underlying thermodynamic mechanisms governing ammonia and hydrazine formation at the water-Fe 3 O 4 -nanoparticle interface. Here, we find that, unlike pure Fe 3 O 4 where N 2 can only interact with a limited number of Fe sites, hydroxylated species introduce large and diverse adsorption geometries where N 2 can bind through either Fe sites or Fe-OH groups, each of which are capable of independently facilitating proton-coupled electron transfer.

Chandy, Sruthy K. [University of California, Berke↗

DOE OSTI2024

General synthesis of high-entropy single-atom nanocages for electrosynthesis of ammonia from nitrate

Given the growing emphasis on energy efficiency, environmental sustainability, and agricultural demand, there’s a pressing need for decentralized and scalable ammonia production. Converting nitrate ions electrochemically, which are commonly found in industrial wastewater and polluted groundwater, into ammonia offers a viable approach for both wastewater treatment and ammonia production yet limited by low producibility and scalability. Here we report a versatile and scalable solution-phase synthesis of high-entropy single-atom nanocages (HESA NCs) in which Fe and other five metals-Co, Cu, Zn, Cd, and In-are isolated via cyano-bridges and coordinated with C and N, respectively. Incorporating and isolating the five metals into the matrix of Fe resulted in Fe-C5 active sites with a minimized symmetry of lattice as well as facilitated water dissociation and thus hydrogenation process. As a result, the Fe-HESA NCs exhibited a high selectivity toward NH3 from the electrocatalytic reduction of nitrate with a Faradaic efficiency of 93.4% while maintaining a high yield rate of 81.4 m h -1 mg -1 .

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Abundant ammonia and nitrogen-rich soluble organic matter in samples from asteroid (101955) Bennu

Organic matter in meteorites reveals clues about early Solar System chemistry and the origin of molecules important to life, but terrestrial exposure complicates interpretation. Samples returned from the B-type asteroid Bennu by the Origins, Spectral Interpretation, Resource Identification, and Security–Regolith Explorer mission enabled us to study pristine carbonaceous astromaterial without uncontrolled exposure to Earth’s biosphere. Here we show that Bennu samples are volatile rich, with more carbon, nitrogen and ammonia than samples from asteroid Ryugu and most meteorites. Nitrogen-15 isotopic enrichments indicate that ammonia and other N-containing soluble molecules formed in a cold molecular cloud or the outer protoplanetary disk. We detected amino acids (including 14 of the 20 used in terrestrial biology), amines, formaldehyde, carboxylic acids, polycyclic aromatic hydrocarbons and N-heterocycles (including all five nucleobases found in DNA and RNA), along with ~10,000 N-bearing chemical species. All chiral non-protein amino acids were racemic or nearly so, implying that terrestrial life’s left-handed chirality may not be due to bias in prebiotic molecules delivered by impacts. The relative abundances of amino acids and other soluble organics suggest formation and alteration by low-temperature reactions, possibly in NH 3 -rich fluids. Bennu’s parent asteroid developed in or accreted ices from a reservoir in the outer Solar System where ammonia ice was stable.

79 ASTRONOMY AND ASTROPHYSICS↗

DOE OSTI2024

Electrodialysis and nitrate reduction (EDNR) to enable distributed ammonia manufacturing from wastewaters

Underutilized wastewaters containing dilute levels of reactive nitrogen (Nr) can help rebalance the nitrogen cycle. This study describes electrodialysis and nitrate reduction (EDNR), a reactive electrochemical separation architecture that combines catalysis and separations to remediate nitrate and ammonium-polluted wastewaters while recovering ammonia. By engineering operating parameters (e.g., background electrolyte, applied potential, electrolyte flow rate), we achieved high recovery and conversion of Nr in both simulated and real wastewaters. The EDNR process demonstrated long-term robustness and up-concentration that recovered >100 mM ammonium fertilizer solution from agricultural runoff that contained 8.2 mM Nr. EDNR is the first reported process to our knowledge that remediates dilute real wastewater and recovers ammonia from multiple Nr pollutants, with an energy consumption (245 MJ per kg NH 3 –N in simulated wastewater, 920 MJ per kg NH 3 –N in agricultural runoff) on par with the state-of-the-art. Demonstrated first at proof-of-concept and engineered to technology readiness level (TRL) 4–5, EDNR shows great promise for distributed wastewater treatment and sustainable ammonia manufacturing.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Simultaneous occupancy of Cu C and Cu D in the ammonia monooxygenase active site

Ammonia monooxygenase (AMO), a copper-dependent membrane enzyme, catalyzes the first and rate-limiting step of nitrification: the oxidation of ammonia to hydroxylamine. Despite its central role in the global nitrogen cycle and its biotechnological relevance, structural characterization of AMO has lagged behind that of its homolog, particulate methane monooxygenase (pMMO), due to the slow growth rates of ammonia-oxidizing bacteria and the instability of AMO upon purification. Recent cryoEM studies of Nitrosomonas europaea AMO and Methylococcus capsulatus (Bath) pMMO in native membranes revealed new structural features, including two adjacent copper-binding sites in the transmembrane region, Cu C and Cu D , believed to constitute the active site. Although multiple structures were determined under various conditions, simultaneous occupancy of Cu C and Cu D was never observed, leaving their potential functional interplay unresolved. Here we report the 2.6 Å resolution cryoEM structure of AMO from Nitrosospira briensis C-128 in isolated native membranes. This structure reveals the first instance of simultaneous copper occupancy of the Cu C and Cu D sites, along with occupancy of the periplasmic Cu B site. Electron paramagnetic resonance (EPR) spectroscopic data indicate that the Cu B site is primarily occupied by Cu(II), while Cu C and Cu D are primarily occupied by diamagnetic ions, presumably Cu(I). Notably, a lipid molecule is bound between the Cu C and Cu D sites, separating them by ∼8.0 Å. The results underscore the importance of studying these enzymes in their native environments across species to resolve conserved and divergent molecular features.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Structures of methane and ammonia monooxygenases in native membranes

Methane- and ammonia-oxidizing bacteria play key roles in the global carbon and nitrogen cycles, respectively. These bacteria use homologous copper membrane monooxygenases to accomplish the defining chemical transformations of their metabolisms: the oxidations of methane to methanol by particulate methane monooxygenase (pMMO) and ammonia to hydroxylamine by ammonia monooxygenase (AMO), enzymes of prime interest for applications in mitigating climate change. However, investigations of these enzymes have been hindered by the need for disruptive detergent solubilization prior to structure determination, confounding studies of pMMO and precluding studies of AMO. Here, we overcome these challenges by using cryoEM to visualize pMMO and AMO directly in their native membrane arrays at 2.4 to 2.8 Å resolution. These structures reveal details of the copper centers, numerous bound lipids, and previously unobserved components, including identifiable and distinct supernumerary helices interacting with pMMO and AMO, suggesting a widespread role for these helices in copper membrane monooxygenases. Comparisons between these structures, their metallocofactors, and their unexpected protein–protein interactions highlight features that may govern activity or the formation of higher-order arrays in native membranes. The ability to obtain molecular insights within the native membrane will enable further understanding of these environmentally important enzymes.

Science & Technology - Other Topics↗

DOE OSTI2024

Development of 250 kW Ammonia and Hydrogen Industrial Burner Test Facility at the National Energy Technology Laboratory

In an effort to investigate the viability of ammonia and hydrogen as fuels in the industrial heating sector, the Department of Energy’s National Energy Technology Laboratory is developing a 250 kW burner test facility. The pursuit of a decarbonized industrial heating sector requires innovative approaches to convert existing assets to alternative fuels while maintaining adequate radiative heat transfer and limiting NOx. This new capability will leverage NETL’s experience and prior investments in ammonia and hydrogen combustion, to advance atmospheric pressure industrial combustion systems for industries such as cement kilns and glass factories. The intention in coming years is to collaborate with burner manufacturers and heavy industry partners to study, develop, and validate strategies for converting existing hardware from carbon-based fuels to next-generation clean ammonia and hydrogen technologies.

May, Kristyn Johnson↗

DOE OSTI2024

Intensification and Integration of Hydrogen and Ammonia Production

In this project the Colorado School of Mines developed a more efficient method for on-site and on-demand generation of high purity hydrogen from ammonia for hydrogen fueling stations. Used primarily as a fertilizer, ammonia is the world’s highest volume commodity chemical. Having 17.6% hydrogen by mass, it also shows potential as a hydrogen carrier and carbon-free fuel. The team developed new technology to generate fuel cell quality hydrogen from ammonia using a catalytic membrane reactor (CMR). In addition, during the project we pivoted to use this CMR technology for the production of NH3/H2 mixtures for use in clean combustion applications. We demonstrated that these mixtures may serve as a drop-in replacement for conventional hydrocarbons such as natural gas. This project entails development of new catalysts, new membranes, and their innovative integration. This project helped generate >$4M in follow on funding at Mines, and resulted in the formation of a clean tech startup, Blaze Energy Technologies, which has licensed IP developed in this project and is working to commercialize this technology.

08 HYDROGEN↗

DOE OSTI2026

Bioinorganic Chemistry of Nitrification: Structure and Function of Ammonia Monooxygenase (Final Technical Report)

The overarching goal of this project was to elucidate biochemical mechanisms that ubiquitous microorganisms use to enable primary metabolism based on nitrification, the multi-electron oxidation of ammonia (NH 3 ) to nitrite (NO 2 – ). This chemistry enables life to substitute carbon based fuel with nitrogen. Understanding the underlying chemistry was pursued to help inform the use of ammonia as an alternative fuel source compared to petroleum, capitalizing on the widespread infrastructure for production and distribution of this substance in the US. This project specifically focused on characterizing ammonia monooxygenase, an integral membrane copper protein that initiates nitrification via the aerobic oxidation of NH 3 to hydroxylamine (NH 2 OH).

09 BIOMASS FUELS↗

NASA NTRS1973

The catalytic removal of ammonia and nitrogen oxides from spacecabin atmospheres

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

Gully, A. J.↗

NASA NTRS1973

Ammonia photolysis on Jupiter.

Ammonia photolysis under simulated Jovian conditions indicates that the photochemical reaction would rapidly convert all the ammonia of Jupiter to nitrogen even in a large excess of hydrogen. It is suggested that ammonia is observed because the planet's atmosphere is deep and hot and/or because electrical discharge phenomena are important.

Nicodem, D. E.↗

NASA NTRS1977

Pyrolysis of organic compounds in the presence of ammonia The Viking Mars lander site alteration experiment

The influence of ammonia on the pyrolysis pattern of selected organic substances sorbed on an inorganic phase was investigated. The thermal degradation products were identified by gas chromatography-mass spectrometry. The feasibility of this technique was tested on a meteoritic sample. All substances examined react with ammonia at the pyrolysis temperature of 500 C, the major products being nitriles and heterocyclic compounds in which nitrogen was incorporated. Based on these results, a model for the non-equilibrium production of organic compounds on Jupiter is discussed. The investigation was performed in connection with the Viking lander molecular analysis. The results obtained indicate that the concentrations of ammonia in the retrorocket fuel exhaust would have been probably too small to produce significant changes in the Martian soil organic compounds if any were found.

Holzer, G.↗

NASA NTRS1980

Reactivity of stratospheric aerosols to small amounts of ammonia in the laboratory environment

Trace ammonia in laboratory air reacts easily with sulfuric acid aerosol samples to form crystalline ammonium sulfate. Argon atmospheres, however, protect sampling surfaces from ammonia contamination. It is found that atmospheric aerosols treated in this way contain only sulfuric acid. After an hour exposed to laboratory air, these same samples convert to ammonium sulfate. Aerosol particles have been collected, using argon control, to determine if the absence of crystalline sulfate is common. But so far there is no evidence that aerosols are neutralized by ammonia in the stratosphere.

Hayes, D.↗

NASA NTRS1982

Stability of ammonia in the primitive terrestrial atmosphere

The rate at which ammonia would have been destroyed in the earth's atmosphere under assumed NH3 mixing ratio conditions of 10 to the -8th to 0.0001 is calculated by a one-dimensional photochemical model, and the destruction rates are compared with possible biotic and abiotic ammonia sources. It is found that, while the mixing ratio of 10 to the -8th needed for the evolution of life could have been maintained by abiotic sources, the value of 0.00001 needed for the production of significant greenhouse warming could not have been sustained abiotically. The increase of atmospheric ammonia due to biological activities during the Archean is also considered lower than the level required for the generation of measurable thermal effects.

Kasting, J. F.↗

NASA NTRS1982

The Jovian ammonia abundance from interferometric observations of limb darkening at 3.4 mm

The relative abundances of the various atomic and molecular constituents in the Jovian atmosphere are important data for studies of the origin of the solar system. The determination of the ammonia abundance presents a number of difficulties. However, difficulties related to a use of the microwave sensing technique can be largely overcome by measuring the brightness distribution across the disk. In particular, information about the atmosphere can be obtained from the degree of limb darkening, which requires only a relative brightness measurement as opposed to an absolute measurement. Valdes and Welch (1978) have used the considered approach in a study of Jupiter at 1.3 cm. In the present investigation a more general relation between the amount of limb darkening in the broad 1.25-cm inversion band of ammonia and the ammonia abundance is derived. The model is applied to new measurements of Jupiter's limb darkening at 3.4 mm.

Valdes, F.↗

NASA NTRS1982

Sources of atmospheric ammonia

The information available on factors that influence emissions from the principal societal sources of ammonia to the atmosphere, namely combustion processes, volatilization of farm animal wastes, and volatilization of fertilizers, is reviewed. Emission factors are established for each major source of atmospheric ammonia. The factors are then multiplied by appropriate source characterization descriptors to obtain calculated fluxes of ammonia to the atmosphere on a state-by-state basis for the United States.

Harriss, R. C.↗

NASA NTRS1984

Production of ammonia-depleted surface layers on the Saturnian satellites by ion sputtering

On the basis of laboratory-derived data on the ion erosion of water and ammonia ices, it is suggested that the surfaces of the Saturnian satellites Enceladus, Tethys, Dione, and Rhea could have become enriched with water ice over a reasonable geological time period owing to the preferential erosion of the ammonia by magnetosphere ion bombardment. This mechanism serves as an alternative explanation to other processes invoked for the absence of ammonia spectral features in these satellites.

Lanzerotti, L. J.↗

NASA NTRS1986

New interstellar masers in nonmetastable ammonia

The first astronomical detections of several ammonia inversion transitions involving nonmetastable levels with energies as high as 1090 K above the ground state are reported. The (J, K) = (9, 6) inversion transition shows maser-like emission in the directions of W51, NGC 7538, W49, and DR 21(OH). The NH3 (6, 3) line exhibits similar characteristics in W51 but is seen in absorption in NGC 7538. These are the first definite detections of ammonia masers in space. The intensities and narrow line widths (0.5-1.5 km/s) for the emission features are in contrast to the previously detected broad, weak, nonmetastable lines attributed to thermal emission in these sources. Temporal variability appears to be evident in the (9, 6) emission in W49 over a 4 month period. The highly excited (J, K) = (9, 6) and (6, 3) ammonia lines are found in regions containig compact H II regions and strongly infrared sources with associated H2O and OH masers; i.e., in regions of active star formation.

Madden, S. C.↗