A golden period for environmental soil chemistry
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99 GENERAL AND MISCELLANEOUS↗
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Grain boundary widening controls siderite (FeCO3) replacement of limestone (CaCO3)
Abstract The microstructure of minerals and rocks can significantly alter reaction rates. This study focuses on identifying transport paths in low porosity rocks based on the hypothesis that grain boundary widening accelerates reactions in which one mineral is replaced by another (replacement reaction). We conducted a time series of replacement experiments of three limestones (CaCO 3 ) of different microstructures and solid impurity contents using FeCl 2 . Reacted solids were analyzed using chemical imaging, small angle X-ray and neutron scattering and Raman spectroscopy. In high porosity limestones replacement is reaction controlled and complete replacement was observed within 2 days. In low porosity limestones that contain 1–2% dolomite impurities and are dominated by grain boundaries, a reaction rim was observed whose width did not change with reaction time. Siderite (FeCO 3 ) nucleation was observed in all parts of the rock cores indicating the percolation of the solution throughout the complete core. Dolomite impurities were identified to act as nucleation sites leading to growth of crystals that exert force on the CaCO 3 grains. Widening of grain boundaries beyond what is expected based on dissolution and thermal grain expansion was observed in the low porosity marble containing dolomite impurities. This leads to a self-perpetuating cycle of grain boundary widening and reaction acceleration instead of reaction front propagation.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Innovative Biomonitoring and Remediation of Heavy Metals Using Phytotechnologies at the Savannah River Site (SRS) Coal Combustion Product (CCP) Impoundment Sites
The Savannah River Site (SRS) contains legacy coal combustion product (CCP) impoundments that are impacted by elevated concentrations of heavy metals and radionuclides, posing long-term risks to soil health, ecosystem functioning, and environmental sustainability. Traditional environmental monitoring approaches rely primarily on chemical analyses to quantify contaminant concentrations but often provide limited information regarding biological responses or ecosystem recovery. This project addressed these limitations by integrating environmental chemistry, microbial ecology, artificial intelligence (AI), and bioremediation into a comprehensive framework for environmental diagnostics and restoration of contaminated soils. The overarching goal of this collaborative project between Florida A&M University (FAMU) and the University of Georgia's Savannah River Ecology Laboratory (SREL) was to develop innovative biomonitoring and remediation strategies for heavy metal-contaminated CCP impoundment sites at the Savannah River Site. Specifically, the project sought to (i) characterize heavy metal contamination, (ii) determine microbial responses to contamination, (iii) isolate indigenous heavy metal-resistant microorganisms for remediation applications, (iv) develop a microbial ecological health index using machine learning, and (v) optimize fungal-mediated bioremediation using artificial intelligence.
01 COAL, LIGNITE, AND PEAT↗
Exploring the Nature of f-Element Soft Donor Interactions Using Electronically Tunable Azolate Ionic Liquids
This project was undertaken to advance the understanding of how f-elements interact with moderately soft donors, a heavily investigated yet open question which is of prime importance in spent nuclear fuel processing and fundamental inorganic chemistry. During the course of the project, based on exciting results, a stretch goal was developed to study the hydrolysis products of transuranic actinide metals, a somewhat understudied field even with its significance in nuclear fuel cycle and impacts in environmental chemistry. The stretch goal was to take our serendipitous discovery of an easy route to isolation of crystalline multinuclear ƒ-element hydrolysis products, and apply it to gaining a mechanistic understanding of Pu(III/IV) colloid formation. The simplicity of our techniques should lend themselves to the remote handling required for study of many transuranic elements. We developed several methodologies using azolium azolate chemistry to overcome ƒ-element hydrolysis problems that prohibit the isolation of ƒ-element soft donor complexes and to build a crystallographic library of ƒ-element N-donor complexes as a means to understand the fundamental differences between actinide and lanthanide interactions with moderately soft donor ligands. Our next major endeavor will be to transfer this chemistry from 4ƒ elements to transuranic elements, particularly in the study of hydrolysis of Pu(III/IV). While our work is fundamental in nature, applications of the knowledge we are generating should be felt in such diverse fields as catalysis, separations in general, nuclear waste remediation specifically, and many other applications in f-element magnetic and luminescent properties. The potential ramifications of the consistent and robust formation of hydrolysis controlled hexanuclear lanthanide structures are enormous, with future uses being catalyst formation, higher-nuclearity structure synthesis using our hexanuclear motif as a fundamental building block, Pu waste remediation, separations, and many other potential applications resulting from characteristic magnetic and luminescent properties of lanthanide polynuclear structures. Three synthetic methodologies (direct mixing with variable stoichiometries, use of volatile solvent, metathesis) were developed starting with 7 acidic and 6 basic azoles to obtain ionic liquids suitable for f-element coordination. Proton transfer by acidic/basic azole combination led to suitable low melting salts and two cocrystals. Acid/base reaction of azoles with soft-donor permanent cations of ([X 4444 ][OH] (where [X 4444 ] + = tetrabutylammonium [N 4444 ] + or tetrabutylphosphonium [P 4444 ] + ) with weakly acidic azoles including imidazole, 1,2,3-triazole, 1,2,4-triazole, 5-aminotetrazole, 4,5-dicyanoimidazole, and 2-amino-4,5-dicyanoimidazole) revealed several suitable low-melting salts. Metathesis reactions of Na(azolate) were conducted by first using weakly acidic azoles including 4,5-dicyanoimidazole, 2-amino-4,5-dicyanoimidazole, 5-aminotetrazole, and 1,2,4-triazole to form sodium or lithium salts using group(I) hydroxides in methanolic solutions. The best results were obtained by reacting the basic and acidic azoles directly in 1:1 or 3:1 ratios at elevated temperatures. Twenty-two azole mixtures were identified which are either low melting solids or room temperature liquids. Each of the low melting solids was confirmed to be a new solid phase, each of which is being further characterized. The liquids and solids are anticipated to be ILs, eutectics, or partially ionized systems, all of which will be suitable for the dissolution of f-element salts. Five new synthetic methodologies were developed to finding suitable crystallization conditions for f-element complexation with the goal of finding simple one pot reaction syntheses and crystallization strategies that could be used under the demanding conditions of transuranic chemistries. These synthetic methods yield many new crystalline phases which were studied by single crystal X-ray diffraction.
12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
Accessibility and Reactivity of Pentavalent Plutonium under Alkaline Conditions
Plutonium exhibits a particularly complex and rich aqueous chemistry due to a dynamic redox equilibrium that can result in the coexistence of four different oxidation states in aqueous solution. Within this equilibrium, pentavalent plutonium is among the most soluble and dominant oxidation states of Pu in neutral to alkaline aqueous solutions of relevance to environmental chemistries and the extreme chemical environments encountered in high-level radioactive wastes. Despite this, the fundamental chemistry of Pu(V) under such conditions remains poorly understood. Here, in this study, we demonstrate the redox accessibility of Pu(V) in alkaline media based on the observations of an electrochemically reversible Pu(VI/V) couple at E 1/2 = 0.19 V vs Hg/HgO (0.29 V vs NHE), allowing us to electrolytically generate Pu(V) in alkaline solution. These Pu(V) solutions remained stable under ambient conditions for at least 9 days before precipitation of crystalline Na 2 [Pu V O 2 (OH) 3 ]·2H 2 O, the first structurally characterized Pu(V) hydroxide. The modest potential of the Pu(VI/V) redox couple allowed us to reproduce Na 2 [Pu V O 2 (OH) 3 ]·2H 2 O synthetically as well as isolate two additional novel Pu(V)-bearing hydroxide phases Na[Pu V O 2 (OH) 2 (H 2 O)]·2.5H 2 O and K 2 [Pu V O 2 (OH) 3 ]·2H 2 O as single crystals from alkaline reactions under mild hydrothermal conditions (<200 °C) using Na 2 O 2 and KO 2 as reductants. This reactivity is rationalized and informed by our electrochemical measurements. The properties of the Pu(V) solids were further characterized by using vibrational and optical spectroscopy.
Kravchuk, Dmytro V. [Argonne National Laboratory (↗
Scanning Electrochemical Microscopy: An Evolving Toolbox for Revealing the Chemistry within Electrochemical Processes
The parallel development of ultramicroelectrodes (UMEs) and groundbreaking scanning probe microscopy techniques in the late 1980s led to the development of the scanning electrochemical microscope. Scanning electrochemical microscopy (SECM) was born from the idea of using a tiny electrode to measure the local electrochemical behavior at operating electrodes. From its foundations, the technique displayed an inherent versatility in measuring sample properties beyond topography. It allowed experimenters to measure and map chemical reactions occurring at diverse interfaces, from inspecting the reversibility of redox mediators at metal electrodes, to detecting the hallmarks of cellular respiration on living plant leaves. Related but distinct electrochemical scanning probe techniques, such as electrochemical atomic force microscopy (EC-AFM), scanning ion conductance microscopy (SICM), and scanning electrochemical cell microscopy (SECCM) have developed in parallel. These techniques have demonstrated exquisite spatial resolution down to the nanoscale regime. However, it is the proposition of this review that SECM remains unmatched at revealing the chemical aspects of electrochemistry. Furthermore, it is our intention to review and demonstrate that the versatile architecture of SECM continues to evolve and address fundamental and emerging challenges in the fields of energy storage and conversion, chemical biology, materials science, and environmental chemistry, among others.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Iron (IV) Formation and the pH Dependent Kinetics of the Fenton Reaction
Despite its widespread importance for biological and environmental chemistry and decades of study, the mechanism underlying the Fenton reaction is still a matter of some controversy. Here, to elucidate the pH dependence of this complex reaction, a new kinetic model is developed to explain the increase in rate and mechanistic shift that occurs from acidic to neutral conditions. This mechanism originated from a re-analysis of a previously proposed model, which neglected explicit iron speciation, leading to unrealistic rate constants. Accounting for speciation suggests a much faster formation rate of Fe(IV), which is estimated to be on the order of 10 6 M −1 s −1 . Expanding on prior kinetic studies that include speciation under acidic conditions, we propose a unified kinetic model that captures the pH-dependent rate acceleration in Fe(II) oxidation by H 2 O 2 , which is a significant step toward resolving the long-standing mechanistic ambiguity of Fenton chemistry.
Cohen, Liron [Lawrence Berkeley National Laborator↗
Novel gas exposure system for the controlled exposure of plants to gaseous hydrogen fluoride
Abstract Plants can serve as sensitive bioindicators of the presence of contaminant vapors in the atmosphere. This work describes a novel laboratory-based gas exposure system capable of calibrating plants as bioindicators for the detection and delineation of the atmospheric contaminant hydrogen fluoride (HF) as a preparatory step for monitoring release emissions. To evaluate changes in plant phenotype and stress-induced physiological effects attributed to HF alone, the gas exposure chamber must have additional controls to simulate otherwise optimal plant growth conditions including variables such as light intensity, photoperiod, temperature, and irrigation. The exposure system was designed to maintain constant growth conditions during a series of independent experiments that varied between optimal (control) and stressful (HF exposure) conditions. The system was also designed to ensure the safe handling and application of HF. An initial system calibration introduced HF gas into the exposure chamber and monitored HF concentrations by cavity ring-down spectroscopy for a 48-h period. Stable concentrations inside the exposure chamber were observed after approximately 15 h, and losses of HF to the system ranged from 88 to 91%. A model plant species ( Festuca arundinacea ) was then exposed to HF for 48 h. Visual phenotype stress-induced responses aligned with symptoms reported in the literature for fluoride exposure (tip dieback and discoloration along the dieback transition margin). Fluoride concentrations in exposed tissues compared to control tissues confirmed enhanced fluoride uptake due to HF exposure. The system described herein can be applied to other reactive atmospheric pollutants of interest in support of bioindicator research.
54 ENVIRONMENTAL SCIENCES↗
Time-resolved electrical potential pump – X-ray photoelectron spectroscopy probe developments for investigating dynamic processes occurring at electrochemical interfaces
Electrode–electrolyte interfaces are of critical importance in several fields, including renewable energy, corrosion, and environmental chemistry. However, investigating these interfaces under operational conditions poses considerable challenges due to the limitations of the instrumentation employed. While recent advancements in in situ and operando techniques have enhanced our comprehension of the steady-state properties of solid-liquid interfaces, the dynamic behaviors of these systems remain inadequately explored. This study introduces a time-resolved X-ray photoelectron spectroscopy (XPS) technique designed to capture transient reaction intermediates and charging dynamics at electrified interfaces. The presented proof-of-principle study demonstrates that electrochemical processes, represented by an equivalent electrical circuit (EEC) model, can be probed and understood using square wave voltage pulses of a potentiostat synchronized to the modified data acquisition of an XPS setup. This method offers a valuable alternative to traditional pump–probe techniques, facilitating the investigation of a broader range of electrochemical systems. A dedicated software package for analyzing time- and energy-resolved XPS with a focus on extracting parameters of the EEC is geared towards benchmarking different EECs in future real-world electrochemical experiments.
Electrochemistry↗
Near-Quantitative Predictions of the First-Shell Coordination Structure of Hydrated First-Row Transition Metal Ions Using K-Edge X-ray Absorption Near-Edge Spectroscopy
Understanding the solvation structure of transition metal ions is important due to its broad impact on the kinetics, stability, and reactivity in a variety of applications in geochemistry, biochemistry, energy storage, and environmental chemistry. Using water as the common ligand, we study the X-ray absorption pre-edge and near-edge spectra at the K-edge of a near-complete series of hydrated first-row transition metal ions with d-orbital occupancy ranging from d 2 to d 10 . Starting with optimized structures that were derived from an explicit solvation treatment at the density functional theory (DFT) level, we then compute the pre-edge X-ray absorption spectra at the metal ion K-edge at the time dependent density functional theory (TDDFT) and restricted active-space second-order perturbation theory (RASPT2) levels of theory. TDDFT calculations provide accurate results for spectra that are dominated by single excitations, while significant improvements were obtained with RASPT2 calculations that correctly distinguish between singly and doubly excited states, where relevant, with quantitative accuracy compared with experiment. We analyze and assign the dierent pre-edge features for each metal ion in order to reveal the impact of the variations in the d orbital occupancy on the rst-shell coordination environment. For completeness, we also report the lowest energy ligand-field d-d transitions for all the transition metal aqua ions considered in this study using complete active space second order perturbation theory (CASPT2).
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Unraveling pH-Dependent Changes in Adsorption Structure of Uranyl on Alumina (012)
Mitigating uranium transport in groundwater is imperative for ensuring access to clean water across the globe. Here, in situ resonant anomalous X-ray reflectivity is used to investigate the adsorption of uranyl on alumina (012) in acidic aqueous solutions, representing typical U VI concentrations of contaminated water near mining sites. The analyses reveal that U VI adsorbs at two distinct heights of 2.4-3.2 and 5-5.3 angstrom from the surface terminal oxygens. The former is interpreted as the mixture of inner-sphere and outer-sphere complexes that adsorb closest to the surface. The latter is interpreted as an outer-sphere complex that shares one equatorial H 2 O with the terminal surface oxygen. With increasing pH, we observe an increasing prevalence of these outer-sphere complexes, indicating the enhanced role of the hydrogen bond that stabilizes adsorbed uranyl species. Finally, the presented work provides a molecular-scale understanding of sorption of uranyl on Al-based-oxide surfaces that has implications for environmental chemistry and materials science.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Light-driven C–H activation mediated by 2D transition metal dichalcogenides
C–H bond activation enables the facile synthesis of new chemicals. While C–H activation in short-chain alkanes has been widely investigated, it remains largely unexplored for long-chain organic molecules. Here, we report light-driven C–H activation in complex organic materials mediated by 2D transition metal dichalcogenides (TMDCs) and the resultant solid-state synthesis of luminescent carbon dots in a spatially-resolved fashion. We unravel the efficient H adsorption and a lowered energy barrier of C–C coupling mediated by 2D TMDCs to promote C–H activation and carbon dots synthesis. Our results shed light on 2D materials for C–H activation in organic compounds for applications in organic chemistry, environmental remediation, and photonic materials.
36 MATERIALS SCIENCE↗
The influence of exploration activities of a potential lithium mine to the environment in Western Serbia
The proposed exploitation of the Jadar Valley lithium/borate deposit in Serbia, by the Rio Tinto Corporation, indicates that it would become large-scale processing of boron- and lithium-containing ore. It would be one of the world’s very first lithium mines in populated and agricultural area. The company claims that the envisioned mining will be in accordance with environmental protection requirements. The Jadar Valley deposits have been claimed to cover 90% of Europe’s current lithium needs. Yet, local opposition to the mining has arisen due to potential devastating impacts on groundwater, soil, water usage, biodiversity loss, and waste accumulation. Research drilling by the mining company has already produced environmental damage, with mine water containing high levels of boron leaking from exploratory wells and causing crops to dry out. Furthermore, our investigations reveal substantially elevated downstream concentrations of boron, arsenic, and lithium in nearby rivers as compared to upstream regions. Additionally, here we show that soil samples exhibit repeated breaches of remediation limit values with environmental consequences on both surface and underground waters. With the opening of the mine, problems will be multiplied by the tailings pond, mine wastewater, noise, air pollution, and light pollution, endangering the lives of numerous local communities and destroying their freshwater sources, agricultural land, livestock, and assets.
54 ENVIRONMENTAL SCIENCES↗
Landuse and land cover shape organic contaminants distribution in the Oconee River watershed in Georgia
Amid growing concerns over the persistence of organic contaminants, this study examines the influence of land-use patterns on their distribution in the Oconee River watershed, Georgia. Surface water samples from five sites across urban, recreational, and forested areas of Georgia’sOconee River watershed were analyzed for 22 organic contaminants, including pesticides and polycyclic aromatic hydrocarbons. Contaminant concentrations varied, with Acenaphthene (max: 19,462.04 ng/L), Chrysene (max: 984.10 ng/L), and Naphthalene (max: 2428.06 ng/L) being predominant. Atrazine (max: 171.04 ng/L) and Malathion (max: 114.99 ng/L)were the most detected pesticides. Land use and land cover significantly influence organic contaminant distribution, with higher levels in forested and urban areas. Risk Quotient (RQ) analysis confirmed no contaminants surpassed the critical threshold, though cumulative exposure may pose long-term risks. The study emphasizes the need for targeted monitoring and regulatory efforts to safeguard water quality in river systems influenced by diverse land-use practices.
54 ENVIRONMENTAL SCIENCES↗
Comprehensive Chemical Fingerprinting by Multidimensional GC and Supervised Machine Learning
This project leveraged advances in machine learning based data analysis techniques and untargeted analytical methods for organic analysis to progress nuclear nonproliferation technologies beyond current capabilities. The developed approaches can be used to detect and identify complex chemical fingerprints of facilities of interest. These techniques have been developed for fields such as metabolomics and genomics but have not been applied to nuclear nonproliferation applications. Adaptation of these techniques for volatile organic compound analysis has far reaching application within the scientific community including environmental chemistry, atmospheric physics, and climate sciences.
98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗
Application of Atmospheric Gases and Particulate Matter to the Assessment of Urban Heat Island
Background: Urban heat island (UHI), where built areas are warmer compared to non-urban regions, increases human related diseases and mortality. A key challenge in UHI analysis is the designation of sites as urban or suburban/rural; however, the growing complexity of green spaces in urban areas and the predominance of the transportation sector in nonurban areas creates a dilemma for distinct delineation. Objectives: This study aims to utilize the variability of atmospheric components such as particulate matter (PM), inorganic gases, and volatile organic compounds (VOCs) as direct tracers of the degree of urbanization for ground-based measurements to fully comprehend UHI in convoluted regions with indistinct delineation of urban and nonurban environments. Methods: Atmospheric gases and aerosols were used as direct tracers of urbanization for UHI analysis. Inorganic gases and particulate matter were monitored in two sites in a southeastern US city with varying degrees of urbanization. VOCs were analyzed using a proton transfer reaction time-of-flight mass spectrometer. Results: The more-urbanized site exhibited warmer night conditions and elevated total oxidant levels, leading to the formation of nanometer-sized particles. Machine learning analysis revealed similar atmospheric pollutant profiles for both sites, suggesting comparable sources and variability. Biogenic VOCs were enhanced at the less-urbanized site; however, levels of anthropogenic aromatic VOCs were comparable for both sites. A comprehensive mass spectra analysis revealed distinct molecular backbones per site that further affirmed the applicability of VOCs as indicators of urbanization. Conclusion: This study concludes that VOCs provide more direct and accurate information than typical inorganic gases and PM parameters for characterizing the degree of urbanization. Further exploration of VOCs can enhance our understanding of UHI dynamics and its interaction with vegetation in urban green spaces.
Air quality sensor↗
Effects of Copolymer Structure on Enzyme-Catalyzed Polyester Recycling
Polyesters are an omnipresent material used for a variety of applications (e.g., bottles, packaging, textile, windshield), roughly comprising 8% of plastics produced worldwide. Enzymatic recycling is an emerging solution to deal with the increasingly diverse polyesters that are not suitable for mechanical recycling. However, enzyme activity and efficiency are still the limiting factors impeding enzymatic recycling for different plastic waste forms. The effects of thermal and structural properties (e.g., glass transition temperature, crystallinity, specific surface area), which are determined by chemical composition and preprocessing, directly influence enzyme recycling efficiency. This work investigates two extrusion methods (single screw and twin-screw extrusion) to pretreat a range of copolyesters (RPET, PETG, Ecozen, Tritan and PBT) and modify their properties (i.e., glass transition temperature (T g ), crystallinity (%), and molecular weight (M n )). A PET-specific enzyme, leaf-branch compost cutinase (LCC ICCG ), produced from a fed-batch fermentation of Escherichia coli BL21(DE3), was used for the enzymatic depolymerization of different polyesters. Several copolyesters showed improved depolymerization after pretreatment, as measured by rate and amount of monomers produced. Furthermore, those that did not depolymerize were found to have exceptionally high glass transition temperature or percent crystallinity, highlighting the importance of these physical parameters on conversion efficiency.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Synthesis of a novel multifunctional organic–inorganic nanocomposite for metal ions and organic dye removals
In this study, we used solvent assisted mechano-synthesis strategies to form multifunctional organic–inorganic nanocomposites capable of removing both organic and inorganic contaminants. A zeolite X (Ze) and activated carbon (AC) composite was synthesized via state-of-the-art mechanical mixing in the presence of few drops of water to form Ze/AC. The second composite (Ze/L/AC) was synthesized in a similar fashion, however this composite had the addition of disodium terephthalate as a linker. Both materials, Ze/AC and Ze/L/AC, were characterized using scanning electron microscope (SEM), energy-dispersive X-ray spectroscopy (EDS), Powdered X-ray diffraction (P-XRD), Fourier-transform infrared spectrometry (FTIR), Accelerated Surface Area and Porosimetry System (ASAP), and thermal gravimetric analysis (TGA). The SEM–EDS displayed the surface structure and composition of each material. The sodium, oxygen and carbon contents increased after linker connected Ze and AC. The P-XRD confirmed the crystallinity of each material as well as the composites, while FTIR indicated the function groups (C=C, O–H) in Ze/L/AC. The contaminant adsorption experiments investigated the effects of pH, temperature, and ionic strength on the adsorption of methylene blue (MB) and Co(II) for each material. In MB adsorption, the first-order reaction rate of Ze/L/AC (0.02 h -1 ) was double that of Ze/AC (0.01 h -1 ). The reaction rate of Ze/L/AC (4.8 h -1 ) was also extraordinarily higher than that of Ze/AC (0.6 h -1 ) in the adsorption of Co(II). Ze/L/AC composite achieved a maximum adsorption capacity of 44.8 mg/g for MB and 66.6 mg/g for Co(II) ions. The MB adsorption of Ze/AC and Ze/L/AC was best fit in Freundlich model with R 2 of 0.96 and 0.97, respectively, which indicated the multilayer adsorption. In the Co(II) adsorption, the data was highly fit in Langmuir model with R 2 of 0.94 and 0.92 which indicated the monolayer adsorption. These results indicated both materials exhibited chemisorption. The activation energy of Ze/L/AC in MB adsorption (34.9 kJ mol -1 ) was higher than that of Ze/L/AC in Co (II) adsorption (26 kJ mol -1 ).
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗