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At least 55 records · Page 3

Changes in nitrate binding with lanthanides in BLPhen complexes

Preorganized ligands such as bis-lactam-1,10-phenanthroline (BLPhen) offer unique selectivity trends in solvent extraction of rare-earth ions, particularly from aqueous nitrate solutions. However, due to the ligand’s lipophilicity it is experimentally challenging to obtain crystal structures of the corresponding lanthanide (Ln):ligand complexes to describe the local structure of the first coordination shell and the role of the nitrate ions in the organic phase. In this work, we report first principles molecular dynamics (FPMD) simulations of the complexation of trivalent lanthanide ions (La, Nd, and Eu) with the BLPhen ligand in the presence of nitrate ions in the dichloroethane (DCE) solvent. We find that two nitrate anions are present in the first solvation shell and the third nitrate anion is far from the first solvation shell in all three [Ln(BLPhen) 2 ] 3+ complexes examined. Moving along the lanthanide series from La to Nd to Eu, the binding pocket formed by the two BLPhen ligands shrinks in size; as a result, the two nitrate configuration changes from one-monodentate/one-bidentate binding mode for La and Nd to all monodentate for Eu. Meanwhile, the total coordination number drops from 11 for La and Nd to 10 for Eu. More interestingly, the bidentate binding in [La(BLPhen) 2 ] 3+ and [Nd(BLPhen) 2 ] 3+ complexes is highly dynamic, frequently switching to monodentate and back. The FPMD insights into the differing modes and dynamics of nitrates in the first coordination shell will be useful for further atomistic understanding of the complex structure, formation, and stability in the organic phase.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Effect of Groundwater Age and Recharge Source on Nitrate Concentrations in Domestic Wells in the San Joaquin Valley

Nitrate is one of the most abundant contaminants in groundwater globally, in the United States, and in California (CA). We studied well construction information, water chemistry, stable isotopes, and noble gases to understand how groundwater travel time and recharge source and mechanism control nitrate concentrations in domestic wells in the San Joaquin Valley (SJV), CA, a large semiarid, irrigated agricultural region. Using nonparametric statistics, we find a decreasing trend in nitrates with groundwater travel time and well depth. Samples collected from wells that are closer to rivers and that show indications of river water recharge, either low recharge temperature or low δ 18 O signature, have lower concentrations of nitrates than samples with isotopic signatures indicating mixed source or local precipitation recharge. The curbing effect of river water recharge on nitrate concentrations in domestic wells is similar for direct river recharge and water applied as irrigation. This suggests that irrigation with river water also has a diluting effect that reduces the concentration of nitrate found in groundwater. This conclusion supports the idea that flood-managed aquifer recharge may be considered for remediation of groundwater nitrate when designing replenishment of aquifers.

54 ENVIRONMENTAL SCIENCES↗

Persistent Heavy Winter Nitrate Pollution Driven by Increased Photochemical Oxidants in Northern China

Nitrate is an increasingly important component of fine particulate matter (PM2.5) during winter in northern China. Past emission control has been ineffective in reducing winter nitrate. Here, we use extensive observations and a model with state-of-theart nitrogen chemistry to identify the key factors that control the nitrate formation in the heavily polluted North China Plain (NCP). In contrast to the previous view of weak winter photochemistry, we show that the O3 and OH productions are sufficiently high in winter to facilitate fast gas-phase and heterogeneous conversion of NOX to nitrate over the NCP. Increasing O3 and OH productions from higher precursor levels and fast ROX cycling accelerate the nitrate generation during heavy pollution. We find that the 31.8% reduction of NOX emissions from 2010 to 2017 in the NCP lowers surface nitrate by only 0.2% and even increases nitrate in some polluted areas. This is mainly due to the increase of O3 and OH (by~30%), which has subsequently increased the conversion efficiency of NOX to HNO3 (by 38.7%). Future control strategies for the winter haze should also aim to lower photochemical oxidants, via larger and synchronized NOX and VOCs emissions reduction, to overcome the effects of nonlinear photochemistry and aerosol chemical feedback.

Fu, Xiao↗

Adaptive responses of Trichlorobacter lovleyi to nitrite detoxification reveal overlooked contributions of Geobacterales to nitrate ammonification

Abstract Poorly understood microorganisms “short-circuit” the nitrogen cycle via the dissimilatory nitrate reduction to ammonium to retain the element in agricultural lands and stimulate crop productivity. The prevalence of Geobacterales closely related to Trichlorobacter lovleyi in nitrate ammonification hotspots motivated us to investigate adaptive responses contributing to ammonification rates in the laboratory type strain T. lovleyi SZ. Here, we describe the identification of tightly regulated pathways for efficient nitrate foraging and respiration with acetate, an important intermediate of organic matter degradation that Geobacterales efficiently assimilate and oxidize. Challenging the established dogma that high carbon/nitrate ratios stimulate the reduction of nitrate to ammonium, T. lovleyi doubled rapidly across a wide range of ratios provided nitrate concentrations were low enough to prevent the accumulation of the toxic nitrite intermediate. Yet, excess electrons during hydrogenotrophic growth alleviated nitrite toxicity and stimulated the reduction of nitrate to ammonium even under conditions of severe acetate limitation. These findings underscore the importance of nitrite toxicity in the ammonification of nitrate by Geobacterales and provide much needed mechanistic understanding of microbial adaptations contributing to soil nitrogen conservation. This information is critical to enhance the predictive value of genomic-based traits in environmental surveys and to guide strategies for sustainable management of nitrogen fertilization as well as mitigation of green-house emissions and agrochemical leaching from agricultural lands.

Environmental Sciences & Ecology↗

Fischer-Tropsch synthesis: Direct cobalt nitrate reduction of promoted Co/Al 2 O 3 catalysts

Direct reduction of cobalt nitrate versus conventional calcination/reduction treatment was conducted using alumina with identical methodology as previously applied to SiO 2 and TiO 2 . Similar BET surface areas, pore volumes and pore size distributions were obtained for the activated calcined and uncalcined catalysts indicating no significant difference on morphological properties. However, the reducibility slightly increases and Co crystallite size is smaller for activated uncalcined samples. Reduction phenomena were analyzed by TPR-MS and TPR-EXAFS/XANES. Combining these techniques allows an explanation of the complex phenomena occurring during the direct reduction of cobalt nitrate, as both nitrate decomposition and cobalt oxide reduction are involved. Cobalt nitrate species are converted to CoO x intermediates. These species are oxidized by NO X (from nitrate decomposition) to Co 3 O 4 spinel, which is converted to CoO prior to Co 0 formation. Noble metals (Pt, Re, Ru and Ag) improve cobalt oxide reducibility, especially for the final reduction step (i.e., CoO to Co 0 ). The effect of direct nitrate reduction on FT activity was investigated using a 1 L CSTR. Activated unpromoted and Pt-promoted uncalcined catalysts achieved higher initial and steady-state CO conversions in comparison to the corresponding calcined catalysts. The best performance was achieved with direct reduction of uncalcined 0.5%Pt-25%Co/Al 2 O 3 .

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Modeled sub-hourly nitrate concentrations in subsurface water across a salt marsh system in Elkhorn Slough, California

Salt marshes are dynamic hydrologic systems where terrestrial groundwater, terrestrial surface water, and seawater mix due to bi-directional flows and pressure gradients. Salt marshes are known to remove excess nitrate from water thereby improving water quality in coastal systems. However, our knowledge of the short-term processes (e.g., intra-tidal) in salt marshes is limited. Further, we lack knowledge about how these short-term dynamics may change as a function of seasonality. To address this knowledge gap, we develope a sampling methodology that allowed us to continuously measure nitrate in subsurface water at three different depths across three marsh elevations at sub-hourly time steps. Here we present a data table with the results of nitrate in porewater across the three salt marsh elevations (information in the data set). We analyzed nitrate with a s::can spectrophotometer. We used the UV-Vis absorbance of the samples to calculate nitrate concentrations using a local calibration library. More information about the methodology can be found in Grande et al (2023). Seasonal and Tidal Variations in Hydrologic Inputs Drive Salt Marsh Porewater Nitrate Dynamics, Hydrological Processes.

54 ENVIRONMENTAL SCIENCES↗

Nitrate loading projection is sensitive to freeze-thaw cycle representation

Climate change can have substantial impacts on nitrogen runoff, which is a major cause of eutrophication, harmful algal blooms, and hypoxia in freshwaters and coastal regions. We examined responses of nitrate loading to climate change in the Upper Mississippi River Basin (UMRB) with an enhanced Soil and Water Assessment Tool with physically based Freeze-Thaw cycle representation (SWAT-FT), as compared with the original SWAT model that employs an empirical equation. Driven by future climate projections from five General Circulation Models (GCMs) from 1960 to 2099 under the Representative Concentrations Pathways (RCP) 8.5 scenario, we analyzed changes in riverine nitrate loadings, as well as terrestrial surface and subsurface contributions of the UMRB in the 21st century relative to the baseline period of 1960–1999. By the end of the 21st century, the original SWAT model predicted about a 50% increase in riverine nitrate loadings which is nearly twice as much as that estimated by SWAT-FT (ca. 25%). Such a large difference in projected nitrate changes can potentially mislead mitigation strategies that aim to reduce nitrogen runoff from the UMRB. Further analysis shows that the difference between the original SWAT model and SWAT-FT led to substantial discrepancies in the spatial distribution of surface and subsurface nitrate loadings in the UMRB. In general, SWAT-FT predicted more nitrate leaching for northwestern parts of the UMRB which are more sensitive to freeze-thaw cycle, mainly because SWAT-FT simulated less frequent frozen soils. This study highlights the importance of using physically based freeze-thaw cycle representation in water quality modeling. Design of future nitrogen runoff reduction strategies should include careful assessment of effects that land management has on the freeze-thaw cycles to provide reliable projection of water quality under climate change.

Wang, Qianfeng↗

Comparison of Gas Phase Fragmentation Behaviors of Nuclear Fuel Cycle Ligands in Lanthanide and Americium Metal Ligand Nitrate Clusters

Title (20 word): Comparison of Gas Phase Fragmentation Behaviors of Nuclear Fuel Cycle Ligands in Lanthanide and Americium Metal Ligand Nitrate Clusters Introduction (120 words): Transport of metal ions across the aqueous-organic phase boundary is an essential step in a hydrometallurgical nuclear fuel reprocessing strategy. The study of transport agents for nuclear fuel elements is imperative to guide the design of ligands that boost the separation efficiency of the recovery process from fission products. However, limited studies have been made on the chemistry of these transport agents when complexing with transuranic elements in gas-phase where all surrounding factors are essentially excluded. This work investigates the reagent ligand complexations to transuranic and other metals and their dissociations in the gas phase. Comparisons are made between 4f and 5f elements and between ligands. Methods (120 words): (N,N-diisobutylcarbamoylmethyl)phenyloctylphosphine oxide (CMPO) and N,N,N',N'-tetraoctyldiglycolamide (TODGA) have been selected to complex with metal nitrates. The actinide americium and lanthanides neodymium, samarium, and europium were investigated as part of this work. The lanthanides were selected to act as size and electron configuration analogues of the minor actinides. Metal complexes with two ligands and two nitrates ([M(NO3)2(CMPO)2]+, for example) are studied in Bruker micrOTOF-Q II mass spectrometer equipped with collision-induced dissociation capability. The comparisons of the mass spectra are made in groups of homogenous ligands and mixed TODGA-CMPO ligands clusters. Comparisons are also made based on the complexed metals (Am and lanthanides). Preliminary data (300 words): Collision-induced dissociation mass spectrometry data are collected on two ligands complexed with metal nitrates where the two ligands are homogenous, with (CMPO)2 or (TODGA)2, or heterogeneous, with (TODGA)(CMPO). Several fragmentation patterns are observed among complexes with the CMPO ligand whereas the TODGA ligand commonly dissociates intact from the complex. Most of the metal complexes exhibit similar fragmentation patterns, but there are a few notable deviations in fragmentation patterns between the Am and Ln-bearing complexes. For the [M(CMPO)2(NO3)2]+ complexes, the initial loss of nitrate in the form of nitric acid is observed in all four complexes. However, [Am(CMPO)2(NO3)2]+ exhibits an additional fragmentation not found in the lanthanide complexes. Also, a significantly different ratio of the second nitric acid loss is found in the Am complex. These deviations may indicate the different interaction behaviors between actinides and lanthanides. The [M(TODGA)2(NO3)2]+ complexes exhibit the fragmentation as the loss of one TODGA ligand as an intact form and the loss of nitrate as nitric acid. The Am complex exhibits an additional fragmentation after losing the TOGDA ligand, which is not observed among the Ln complexes. The heterogeneous [M(TODGA)(CMPO)(NO3)2]+ complexes exhibit both similarities and differences between the Am and Ln complexes. For example, the heterogenous Am complex does not exhibit the loss of an intact TODGA ligand while all three Ln complexes do. This indicates that TODGA may bind more strongly to Am than Ln. Additionally, the intensity of the loss of CMPO ligand (as partially or whole) is found to be significantly larger than that of the loss of TODGA (as partially of whole) indicating that TODGA is bound to the metal significantly stronger than CMPO. Planned computational analysis will help understand the deviation in fragmentation behaviors between americium and lanthanide metal centers, or between TODGA and CMPO ligands. Novel aspect (20 words): Gas-phase actinide and lanthanide complex formation and fragmentation provide insight into the coordination environment differences of f-element metals.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Genetic encoding of 3–nitro–tyrosine reveals the impacts of 14–3–3 nitration on client binding and dephosphorylation

14–3–3 proteins are central hub regulators of hundreds of phosphorylated “client” proteins. They are subject to over 60 post–translational modifications (PTMs), yet little is known how these PTMs alter 14–3–3 function and its ability to regulate downstream signaling pathways. An often neglected, but well–documented 14–3–3 PTM found under physiological and immune–stimulatory conditions is the conversion of tyrosine to 3–nitro–tyrosine at several Tyr sites, two of which are located at sites considered important for 14–3–3 function: Y130 (β–isoform numbering) is located in the primary phospho–client peptide–binding groove, while Y213 is found on a secondary binding site that engages with clients for full 14–3–3/client complex formation and client regulation. By genetically encoding 3–nitro–tyrosine, we sought to understand if nitration at Y130 and Y213 effectively modulated 14–3–3 structure, function, and client complexation. The 1.5 Å resolution crystal structure of 14–3–3 nitrated at Y130 showed the nitro group altered the conformation of key residues in the primary binding site, while functional studies confirmed client proteins failed to bind this variant of 14–3–3. But, in contrast to other client–binding deficient variants, it did not localize to the nucleus. Further, the 1.9 Å resolution structure of 14–3–3 nitrated at Y213 revealed unusual flexibility of its C–terminal α–helix resulting in domain swapping, suggesting additional structural plasticity though its relevance is not clear as this nitrated form retained its ability to bind clients. Collectively, our data suggest that nitration of 14–3–3 will alter downstream signaling systems, and if uncontrolled could result in global dysregulation of the 14–3–3 interactome.

14-3-3↗

Nitrate and Nitrite Incompatibility with Hydroxide Ions in Concentrated NaOH Solutions: Implications for Hydroxide and Gibbsite Reactivity in Alkaline Nuclear Waste

Electrolyte solutions in alkaline nuclear waste contain aluminate, hydroxide, nitrate and nitrite with sodium as the predominant counterion. The salts of these ions are highly soluble, so the liquids are highly concentrated. This study found that there is a substantial incompatibility between the hydroxide and nitrate and/or nitrate ions. This was determined by the observations that adding just one molal of NaNO2 or NaNO3 to saturated NaOH solution precipitation of 12 moles of NaOH·H2O salt, whereas the common ion effect would have expected only about 1 mole to precipitate. Further analysis indicates that the presence of nitrate and nitrite drastically increases the reactivity of sodium hydroxide ions in solution, which likely influences the reactivity of other hydroxide-mediated reactions. This enhanced reactivity is likely because it disrupts large Na+-OH- ion networks because nitrate and nitrite do not fit in those ion networks similarly to how some ions cannot substitute into a foreign crystal lattice. In contrast, the aluminate ion did not have the same large incompatibility with hydroxide.

Nitrite, Nitrate, Aluminate, NaOH*H2O, Ion-aggrega↗

Evaluation of the lgnitability Hazards in Remediated Nitrate Salt Waste

The hazards associated with the characteristic of ignitability in remediated nitrate salt (RNS) waste containing nitric acid (HNO 3 ) and metal nitrate salts, currently stored at the Waste Control Specialists (WCS) facility near Andrews, Texas have been evaluated. For these waste drums there are two ignitability hazards that may apply, each separately distinguished from the other and uniquely correlated to one of two competing reaction mechanisms. One ignitability hazard, designated the autocatalytic thermal runway, is uniquely correlated to an acid/base reaction of hydrolysis of a hydrated metal nitrate salt. The other applicable ignitability hazard, designated the oxidizer property, is uniquely correlated to a redox disproportionation reaction involving an anhydrous metal nitrate salt. Which reaction mechanism pathway is accessible to a given metal nitrate, and therefore which ignitability hazard may apply, depends on the acidity of the metal ion and its corresponding capacity to maintain coordination with water.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Electrocatalytic nitrate reduction: controlling adsorbate affinity to tailor reaction products

Every year, Haber-Bosch nitrogen fixation to form ammonia releases immense volumes of CO2. At the same time, nitrate contamination from untreated wastewater threatens human health across the US. Development of circular processes to efficiently upgrade waste nitrate for reuse is critical to sustainably address this growing environmental hazard. Electrochemical reduction of nitrate operates at ambient temperatures and pressures, and can leverage distributed renewable energy sources and water as a hydrogen source for ammonia production. However, current catalysts lack electron efficiency in reducing nitrate versus water, lack selectivity in forming ammonia as a product, or rely on expensive rare metals, making widespread implementation unfeasible. To overcome these limitations, this proposal seeks a mechanistic understanding of nitrate electrochemical reduction on earth abundant metals and their alloys, with the goal of identifying active-site properties that improve both Faradaic efficiency and product selectivity. This insight will extend to other electrocatalytic reductive process that compete with water reduction.

30 DIRECT ENERGY CONVERSION↗

Investigating Np(VI) Nitrate Speciation Control through Temperature and Optical Spectroscopy

Numerous areas of nuclear processing, such as radioisotope production, nuclear waste remediation, and separations, depend upon the speciation of f-elements in the solution state. However, fundamental knowledge of the actinides─particularly Np─lags behind most of the elements on the periodic table. Despite the importance of Np(VI) chemistry in separations and nuclear processing, its speciation in HNO 3 remains uncertain. This work addresses some of these gaps by investigating the effect of HNO 3 concentration and temperature on the spectra and speciation of the Np(VI) nitrate system. Six samples of Np in 1 to 10 M HNO 3 were prepared and treated with (NH 4 ) 2 [Ce(NO 3 ) 6 ] to stabilize the hexavalent oxidation state. The absorbance spectrum of the 10 M HNO 3 is drastically different from the spectra of the other samples; the 10 M spectrum indicates coordination of nitrate ligands to the Np(VI)O 2 2+ ion to form a complex with high symmetry. Additionally, absorbance spectra were recorded over the temperature range of 15 to 40 °C, and systematic increases and decreases in certain spectral features of the ultraviolet–visible (UV–vis)–near-infrared (NIR) spectra are present in the spectra. The difference in spectral features suggests that Np(VI) nitrate speciation depends on temperature. Dilution studies of this sample were monitored with UV–vis–NIR and Raman spectroscopies. Spectral data indicate the presence of multiple complexes with different symmetries, including a high-symmetry complex with an inversion center. As samples are diluted and aquo ligands replace nitrate ligands bound to the Np(VI) neptunyl cation, changes in spectroscopic signals indicate a decrease in the high-symmetry nitrate complex and an increase in the lower-symmetry aquo complex. Additionally, the Raman band associated with the Np(VI)O 2 2+ symmetric stretch broadens with dilution and is fitted with two peaks. These peaks are assigned to Np(VI) aquo and nitrato complexes, indicating that this vibrational mode is sensitive to the coordination environment of the Np(VI) neptunyl cation and that contributions from these two Np(VI) complexes can be distinguished. This unique experimental data could be used to advance computational models describing the electronic transitions of complex actinyl ions.

Absorption↗

Seasonal and Morphological Controls on Nitrate Retention in Arctic Deltas

Abstract Estimates of nitrate loading to the Arctic Ocean are limited by the lack of field observations within deltas partly due to logistical constraints. To overcome this limitation, we use a remote sensing framework to estimate retention of nitrate in Arctic deltas. We achieve this by coupling hydrological and biogeochemical process models at the network scale for five major Arctic deltas. Binary masks of delta channels were used to simulate flow direction and magnitude through networks. Models were parameterized using historical and seasonal observations. Simulated nitrate retention ranged from 2.9% to 15% of the incoming load. Retention rates were largest during winter but smallest during spring conditions when increased discharges export large nitrate masses to the coast. Under future climate scenarios, retention rates fall by ∼1%–10%. Arctic deltas have an important effect on the magnitude of nitrate entering Arctic seas and the inclusion of processing in deltas can improve flux estimates.

54 ENVIRONMENTAL SCIENCES↗

Controlling solvation in conducting redox polymers for selective electrochemical separation of nitrate from wastewater

Selective capture of nitrate from wastewater is crucial for ensuring safe drinking water and promoting resource circularity. This study investigated alkylated polyaniline redox polymers as highly-selective electrosorbents to address this challenge. By controlling polymer solvation properties through synthetic functionalization, poly(N-methylaniline) (PNMA) achieves a nitrate uptake of up to 1.38 mmol g −1 -polymer and a separation factor of 7 over chloride. Poly(N-butylaniline) (PNBA) further enhances selectivity, achieving a separation factor beyond 14 due to increased hydrophobicity. The mechanisms underlying this selectivity are investigated using ab initio molecular dynamics (AIMD) and in-situ electrochemical quartz crystal microbalance (EQCM) studies, which reveal that hydrophobicity reduces chloride binding. A technoeconomic analysis indicates that methylation on PANI reduces nitrate removal costs by 50% compared to non-functionalized PANI, due to enhanced selectivity and uptake, and decreased energy consumption. PNMA electrodes demonstrate practical nitrate selectivity over 20 versus chloride in real wastewater, while avoiding sulfate binding. This study highlights the potential of controlling solvation at electroactive polymers to enhance nitrate selectivity, offering a promising design path for redox-mediated electrochemical separations.

chemical engineering↗

Comparison of Gas Phase Fragmentation Behaviors of Nuclear Fuel Cycle Ligands in Lanthanide and Americium Metal Ligand Nitrate Clusters

Introduction (120 words): Transport of metal ions across the aqueous-organic phase boundary is an essential step in a hydrometallurgical nuclear fuel reprocessing strategy. The study of transport agents for nuclear fuel elements is imperative to guide the design of ligands that boost the separation efficiency of the recovery process from fission products. However, limited studies have been made on the chemistry of these transport agents when complexing with transuranic elements in gas-phase where all surrounding factors are essentially excluded. This work investigates the reagent ligand complexations to transuranic and other metals and their dissociations in the gas phase. Comparisons are made between 4f and 5f elements and between ligands. Methods (120 words): (N,N-diisobutylcarbamoylmethyl)phenyloctylphosphine oxide (CMPO) and N,N,N',N'-tetraoctyldiglycolamide (TODGA) have been selected to complex with metal nitrates. The actinide americium and lanthanides neodymium, samarium, and europium were investigated as part of this work. The lanthanides were selected to act as size and electron configuration analogues of the minor actinides. Metal complexes with two ligands and two nitrates ([M(NO3)2(CMPO)2]+, for example) are studied in Bruker micrOTOF-Q II mass spectrometer equipped with collision-induced dissociation capability. The comparisons of the mass spectra are made in groups of homogenous ligands and mixed TODGA-CMPO ligands clusters. Comparisons are also made based on the complexed metals (Am and lanthanides). Preliminary data (300 words): Collision-induced dissociation mass spectrometry data are collected on two ligands complexed with metal nitrates where the two ligands are homogenous, with (CMPO)2 or (TODGA)2, or heterogeneous, with (TODGA)(CMPO). Several fragmentation patterns are observed among complexes with the CMPO ligand whereas the TODGA ligand commonly dissociates intact from the complex. Most of the metal complexes exhibit similar fragmentation patterns, but there are a few notable deviations in fragmentation patterns between the Am and Ln-bearing complexes. For the [M(CMPO)2(NO3)2]+ complexes, the initial loss of nitrate in the form of nitric acid is observed in all four complexes. However, [Am(CMPO)2(NO3)2]+ exhibits an additional fragmentation not found in the lanthanide complexes. Also, a significantly different ratio of the second nitric acid loss is found in the Am complex. These deviations may indicate the different interaction behaviors between actinides and lanthanides. The [M(TODGA)2(NO3)2]+ complexes exhibit the fragmentation as the loss of one TODGA ligand as an intact form and the loss of nitrate as nitric acid. The Am complex exhibits an additional fragmentation after losing the TOGDA ligand, which is not observed among the Ln complexes. The heterogeneous [M(TODGA)(CMPO)(NO3)2]+ complexes exhibit both similarities and differences between the Am and Ln complexes. For example, the heterogenous Am complex does not exhibit the loss of an intact TODGA ligand while all three Ln complexes do. This indicates that TODGA may bind more strongly to Am than Ln. Additionally, the intensity of the loss of CMPO ligand (as partially or whole) is found to be significantly larger than that of the loss of TODGA (as partially of whole) indicating that TODGA is bound to the metal significantly stronger than CMPO. Planned computational analysis will help understand the deviation in fragmentation behaviors between americium and lanthanide metal centers, or between TODGA and CMPO ligands. Novel aspect (20 words): Gas-phase actinide and lanthanide complex formation and fragmentation provide insight into the coordination environment differences of f-element metals.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Mild and Selective Hydrogenation of Nitrate to Ammonia in the Absence of Noble Metals

Motivated by increased awareness about nitrate contamination of surface waters and its deleterious effects in human and animal health, we sought an alternative, non-noble metal catalyst for the chemical degradation of nitrate. First row transition metal phosphides recently emerged as excellent alternatives for hydrogen evolution and hydrotreating reactions. We demonstrate that a key member of this family, Ni 2 P, readily hydrogenates nitrate (NO 3 – ) to ammonia (NH 3 ) near ambient conditions with very high selectivity (96%). One of the few non-precious metal-based catalysts for this transformation, and among ca. 1% of catalysts with NH 3 selectivity, Ni 2 P can be recycled multiple times with limited loss of activity. Both nitrite (NO 2 – ) and nitric oxide (NO) intermediates are also hydrogenated. Density functional theory (DFT) indicates that—in the absence of a catalyst—nitrite hydrogenation is the reaction bottleneck. A variety of adsorbates (H, O, N, NO) induce surface reconstruction with top-layer Ni-rich surface stoichiometry. Critically, H saturation coverage on Ni 2 P(001) is only ca. 3 nm –2 , significantly less than that on Pd(111) and Ni(111) of ca. 15–18 nm –2 , which may play a key role in allowing coadsorption of NO x – . Here the ability of Earth-abundant, binary metal phosphides such as Ni 2 P to catalyze nitrate hydrogenation could transform and help us to better understand the basic science behind catalytic hydrogenation and, in turn, advance the next generation of oxyanion removal technologies.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Rapid denitrification of nitrate-contaminated groundwater in a low-gradient blackwater stream valley

Leaching of excess nitrogen (N) to groundwater in fertilized landscapes can overwhelm natural biogeochemical processes and cause long-term eutrophication of aquatic systems. We investigated N fate and transport from an intensively managed short-rotation woody crop (Pinus taeda) plantation through the riparian zone of an intermittent, low-gradient blackwater stream. Fertilization of the P. taeda plantation on the uplands resulted in contamination of groundwater with nitrate concentrations between 0.9 and 1.9 mg N L -1 . No corresponding increase in nitrate was observed in stream water or shallow groundwater in the riparian zone. Groundwater travel-time modeling predicted that N from near-stream, upland plantation areas should have reached streams during the monitoring period. Two years of measuring N species in well water in contrasting landscape positions (within the plantation, swale, riparian edge, forested hillslope, and valley), indicated rapid nitrate transformation and denitrification within the forested wetland valleys. Denitrification in the shallow groundwater system within the toeslopes and the riparian zone was estimated to have removed > 90% of nitrate. Finally, these results highlight the importance of riparian zones as pathways for the removal of N and for controlling downstream N loads.

54 ENVIRONMENTAL SCIENCES↗