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At least 235 records · Page 13
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Effects of flow on uranium speciation in soils impacted by acidic waste fluids

Radioactive acidic liquid waste is a common byproduct of uranium (U) and plutonium (Pu) enrichment and recycling processes whose accidental and planned release has led to a significant input of U into soils and sediments across the world, including at the U.S. DOE's Hanford site (WA, USA). Because of the particularly hazardous nature of U, it is important to predict its speciation when introduced into soils and sediments by acidic waste fluids. Of fundamental importance are the coupled effects of acid-driven mineral transformation and reactive transport on U speciation. To evaluate the effect of waste-fluid residence time and co-associated dissolved phosphate concentrations on U speciation in impacted soils and sediments, uncontaminated surface materials (from the Hanford Site) were reacted with U-containing synthetic acidic waste fluids (pH 2) amended with dissolved phosphate concentrations in both batch (no flow) and flow-through column systems for 7–365 days. By comparing dissolved U behavior and solid phase speciation as a function of flow regimen, we found that the availability of proton-promoted dissolution products (such as Si) to sequester U into uranyl silicates was dependent on waste fluid-sediment contact time as uranyl silicates were not detected in short contact time flow-through systems but were detected in no-flow, long contact time, reactors. Moreover, the dominance of uranyl phosphate as neoprecipitate U scavenger (principally in the form of meta-ankoleite) in phosphate amended systems confirmed the importance of phosphate amendments for an efficient sequestration of U in the soils and sediments. Overall, our experiments suggest that the formation of uranyl silicates in soils impacted by acidic waste fluids is likely to be limited unless reaction products are allowed to accumulate in soil pores, highlighting the importance of investigating soil U speciation in flow-through, transport-driven systems as opposed to no-flow, batch systems. Finally, this study provides insights into uranium speciation and its potential changes under acidic conditions for better prediction of risks and subsequent development of efficient remediation strategies.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2024

Studies on the Vitrification Potential of High Risk Spent Nuclear Fuels

This research explored vitrification of U-Zr nuclear fuel that exhibits an explosion hazard when processed by common nitric acid dissolution. Glass frits were chosen based on properties that had been previously measured as well as being demonstrated successfully in production at the Defense Waste Process Facility (DWPF). Zirconium and Aluminum metal powders were chosen to represent the spent fuels after literature demonstrated that the potential phase that causes the issue for explosive reaction in the effluent stream is tied to the Zirconium-III phase field. DSC measurements were carried out on various simulants and waste forms to better understand thermal behavior of these materials. Zirconium (Zr) was tested with both nitric acid and the new effluent flowsheet that is under development by the SRNL Chemical Process Control (CPC) group. The nitric acid test did show the expected exothermic behavior as well as how the behavior is affected by particle size of the powders used. In contrast, the effluent samples did not show an exothermic peak. However, the concentration of metal in the samples was orders of magnitude lower than in the nitric acid testing and further testing of the effect of concentration on the exothermicity that could be measured confirmed a dampened signal. Tests were run that included frit, both DWPF Frit 510 and Iron Phosphate frit, exhibiting complex curves that included multiple endothermic and exothermic peaks during heating and cooling. The final crucible samples appear similarly to the bulk glasses pointing to these peaks being a part of the dissolution of the simulant into the base glasses.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

Sac1 links phosphoinositide turnover to cryptococcal virulence

Cryptococcus neoformans is an environmentally acquired fungal pathogen that causes over 140,000 deaths per year. Cryptococcal infection occurs when infectious particles are deposited into the lung, where they encounter host phagocytic cells. C. neoformans may be engulfed by these phagocytes, an important step of infection that leads to outcomes ranging from termination of infection to cryptococcal dissemination. To study this critical process, we screened approximately 4,700 cryptococcal gene deletion mutants for altered uptake, using primary mouse and human phagocytic cells. Among the hits of these two screens, we identified 93 mutants with perturbed uptake in both systems, as well as others with differences in uptake by only one cell type. We further screened the hits for changes in thickness of the capsule, a protective polysaccharide layer around the cell which is an important cryptococcal virulence factor. The combination of our three screens yielded 45 mutants, including one lacking the phosphatidylinositol-4-phosphate phosphatase Sac1. In this work, we implicate Sac1 in both host cell uptake and capsule production. We found that sac1 mutants exhibit lipid trafficking defects, reductions in secretory system function, and changes in capsule size and composition. Many of these changes occur specifically in tissue culture media, highlighting the role of Sac1 phosphatase activity in responding to the stress of host-like conditions. Overall, these findings show how genome-scale screening can identify cellular factors that contribute to our understanding of cryptococcal biology and demonstrate the role of Sac1 in determining fungal virulence.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2026

ICL Commercial Production of Lithium Iron Phosphate Cathode Powder for the Global Lithium Battery Industry Final Technical Report

ICL was investing in producing cathode active material, Lithium Iron Phosphate (LFP), used in the production of batteries for both electric vehicles and stationary storage. The demand for LFP was increasing with the global focus on sustainable energy, and there was no current manufacturer of this material in the United States. As such, imported LFP is subject to the uncertainties around supply chain and control of a foreign supplier. This investment would have allowed ICL to be a United States leader in LFP production. To gain a position in this market, ICL licensed the technology from a firm that has the process technology and has reliably supplied LFP into the battery market and currently has customers purchasing their product.

25 ENERGY STORAGE↗
DOE OSTI2022

The mitochondrial Cu + transporter PiC2 (SLC25A3) is a target of MTF1 and contributes to the development of skeletal muscle in vitro

The loading of copper (Cu) into cytochrome c oxidase (COX) in mitochondria is essential for energy production in cells. Extensive studies have been performed to characterize mitochondrial cuproenzymes that contribute to the metallation of COX, such as Sco1, Sco2, and Cox17. However, limited information is available on the upstream mechanism of Cu transport and delivery to mitochondria, especially through Cu-impermeable membranes, in mammalian cells. The mitochondrial phosphate transporter SLC25A3, also known as PiC2, binds Cu + and transports the ion through these membranes in eukaryotic cells, ultimately aiding in the metallation of COX. We used the well-established differentiation model of primary myoblasts derived from mouse satellite cells, wherein Cu availability is necessary for growth and maturation, and showed that PiC2 is a target of MTF1, and its expression is both induced during myogenesis and favored by Cu supplementation. PiC2 deletion using CRISPR/Cas9 showed that the transporter is required for proliferation and differentiation of primary myoblasts, as both processes are delayed upon PiC2 knock-out. The effects of PiC2 deletion were rescued by the addition of Cu to the growth medium, implying the deleterious effects of PiC2 knockout in myoblasts may be in part due to a failure to deliver sufficient Cu to the mitochondria, which can be compensated by other mitochondrial cuproproteins. Co-localization and co-immunoprecipitation of PiC2 and COX also suggest that PiC2 may participate upstream in the copper delivery chain into COX, as verified by in vitro Cu + -transfer experiments. These data indicate an important role for PiC2 in both the delivery of Cu to the mitochondria and COX, favoring the differentiation of primary myoblasts.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2022

Intramolecular carbon isotope signals reflect metabolite allocation in plants

Abstract Stable isotopes at natural abundance are key tools to study physiological processes occurring outside the temporal scope of manipulation and monitoring experiments. Whole-molecule carbon isotope ratios (13C/12C) enable assessments of plant carbon uptake yet conceal information about carbon allocation. Here, we identify an intramolecular 13C/12C signal at tree-ring glucose C-5 and C-6 and develop experimentally testable theories on its origin. More specifically, we assess the potential of processes within C3 metabolism for signal introduction based (inter alia) on constraints on signal propagation posed by metabolic networks. We propose that the intramolecular signal reports carbon allocation into major metabolic pathways in actively photosynthesizing leaf cells including the anaplerotic, shikimate, and non-mevalonate pathway. We support our theoretical framework by linking it to previously reported whole-molecule 13C/12C increases in cellulose of ozone-treated Betula pendula and a highly significant relationship between the intramolecular signal and tropospheric ozone concentration. Our theory postulates a pronounced preference for leaf cytosolic triose-phosphate isomerase to catalyse the forward reaction in vivo (dihydroxyacetone phosphate to glyceraldehyde 3-phosphate). In conclusion, intramolecular 13C/12C analysis resolves information about carbon uptake and allocation enabling more comprehensive assessments of carbon metabolism than whole-molecule 13C/12C analysis.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2022

Global Patterns and Controls of Nutrient Immobilization on Decomposing Cellulose in Riverine Ecosystems

Microbes play a critical role in plant litter decomposition and influence the fate of carbon in rivers and riparian zones. When decomposing low-nutrient plant litter, microbes acquire nitrogen (N) and phosphorus (P) from the environment (i.e., nutrient immobilization), and this process is potentially sensitive to nutrient loading and changing climate. Nonetheless, environmental controls on immobilization are poorly understood because rates are also influenced by plant litter chemistry, which is coupled to the same environmental factors. Here we used a standardized, low-nutrient organic matter substrate (cotton strips) to quantify nutrient immobilization at 100 paired stream and riparian sites representing 11 biomes worldwide. Immobilization rates varied by three orders of magnitude, were greater in rivers than riparian zones, and were strongly correlated to decomposition rates. In rivers, P immobilization rates were controlled by surface water phosphate concentrations, but N immobilization rates were not related to inorganic N. The N:P of immobilized nutrients was tightly constrained to a molar ratio of 10:1 despite wide variation in surface water N:P. Immobilization rates were temperature-dependent in riparian zones but not related to temperature in rivers. However, in rivers nutrient supply ultimately controlled whether microbes could achieve the maximum expected decomposition rate at a given temperature. Collectively, we demonstrated that exogenous nutrient supply and immobilization are critical control points for decomposition of organic matter.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2026

FY25 Ion Exchange Processing for the West Area Risk Management (WARM) Project

The West Area Risk Management (WARM) Project was established to enable near-term retrieval and pretreatment of tank waste from Hanford’s 200 West Area and to support deployment of an ion exchange (IX) system capable of producing cesium-depleted supernate suitable for offsite treatment and disposal. The WARM experimental campaign was designed to provide key data for design and operational planning of the 200 W IX system, which plans to utilize crystalline silicotitanate (CST) as the active media for cesium removal. This report documents a comprehensive FY25 experimental campaign designed to produce key technical data required for design and operational planning of the WARM IX system. Testing includes assessing Cs and Sr breakthrough performance in a 4-column system, Cs capacity batch contact testing, phosphate precipitation assessments, reduced-hydroxide feed displacement evaluation, and Sr speciation impacts on Sr removal. The experimental results provide detailed trends in Cs and Sr loading behavior, breakthrough performance across a 4-column staged IX system, distribution profiles within CST beds, and projections of operational flowrates relative to Waste Acceptance Criteria (WAC) limits. Batch contact testing established equilibrium partitioning behavior for the S1–S5 simulants and characterized how matrix chemistry influenced Cs sorption onto CST. Additionally, further evaluations on waste matrix as it pertains to precipitation potential were also determined. Collectively, these datasets support engineering design choices for WARM system throughput and pretreatment planning.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2020

Electrodeposited Aluminum Oxide as Alternative to Conventional Pretreatments

Iron and zinc phosphate pretreatments are still heavily used in both the oil & gas and automotive industries as adhesion promoters for paints and E-coat systems. These solutions are known to generate hazardous sludges and rinse water which must be periodically disposed of, a problem made worse by the increasing desire for aluminum alloy incorporation in vehicles. This presentation will introduce novel electrodeposited aluminum oxide pretreatments as a sustainable alternative to phosphates. The aluminum oxide coatings improve corrosion resistance and paint adhesion, generate no hazardous waste streams, are cost-effective, and can be applied to any metal surface. This new type of surface pretreatment can conform to TT-C-490 Type IV and VI for Military applications on both ferrous and non-ferrous surfaces as well as automotive specifications for equivalent civilian markets. The thin aluminum oxide treatment also supports the development of lightweight coatings systems for automotive and aerospace applications without sacrificing performance and is a perfect complement to the E-coating process. Since aluminum oxide uses a chemical binding mechanism for paints, the surface can even be modified to offer excellent paint adhesion and corrosion resistance directly to top-coats without the need for primer. This opens a pathway to fewer coating steps for simplified paint application and lightweight, next-generation coatings systems.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Human DNA polymerase η promotes RNA-templated error-free repair of DNA double-strand breaks

A growing body of evidence indicates that RNA plays a critical role in orchestrating DNA double-strand break repair (DSBR). Recently, we showed that homologous nascent RNA can be used as a template for error-free repair of double-strand breaks (DSBs) in the transcribed genome and to restore the missing sequence at the break site via the transcription-coupled classical nonhomologous end-joining (TC-NHEJ) pathway. TC-NHEJ is a complex multistep process in which a reverse transcriptase (RT) is essential for synthesizing the DNA strand from template RNA. However, the identity of the RT involved in the TC-NHEJ pathway remained unknown. Here, we report that DNA polymerase eta (Pol η), known to possess RT activity, plays a critical role in TC-NHEJ. We found that Pol η forms a multiprotein complex with RNAP II and other TC-NHEJ factors, while also associating with nascent RNA. Moreover, purified Pol η, along with DSBR proteins PNKP, XRCC4, and Ligase IV can fully repair RNA templated 3'-phosphate-containing gapped DNA substrate. In addition, we demonstrate here that Pol η deficiency leads to accumulation of R-loops and persistent strand breaks in the transcribed genes. Finally, we determined that, in Pol η depleted but not in control cells, TC-NHEJ-mediated repair was severely abrogated when a reporter plasmid containing a DSB with several nucleotide deletion within the E. coli lacZ gene was introduced for repair in lacZ-expressing mammalian cells. Thus, our data strongly suggest that RT activity of Pol η is required in error-free DSBR.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2023

NMR investigation of proton transport in polybenzimidazole/polyphosphoric acid membranes prepared via novel synthesis route

Here, in this work, we present a molecular-level view of the structural changes in polybenzimidazole (PBI) membranes doped with phosphoric acid (PA) generated by a novel membrane fabrication technique. The modified PA doped membranes displayed unprecedented ionic conductivity at elevated temperatures, comparable to the starting PBI gel membranes prepared by the commonly used PPA process, while also exhibiting enhanced mechanical properties. To elucidate the cause of these effects, we used multi-nuclear ( 1 H, 13 C, 31 P) 1D PFG, MAS and CPMAS, and 2D HETCOR magnetic resonance (NMR) techniques to characterize the structure and dynamics of the modified film and the original gel PBI membranes. 1 H diffusivity measurements show significantly enhanced proton diffusivity, both in magnitude and in lower activation energy, which were consistent with its high ionic conductivity despite the lower PA content compared to the original gel membrane. CPMAS experiments further substantiated that the location of these distinct phosphate environments as being close to the polymer network. Finally, the phosphate groups in the modified membrane were revealed to be strongly bounded to each other and to the PBI polymer backbone in contrast to the combination of weakly and strongly bounded groups of the original gel membrane.

74 ATOMIC AND MOLECULAR PHYSICS↗
DOE OSTI2022

Adrian Portales Coop Internship Report

Using the thesis of W.R. Nolan (cite) as a guide, Cobalt Iron (CoFe) powders were reacted with 0.1 wt.% and 0.2 wt.% phosphoric acid in a 20:1 ratio of acetone to phosphoric acid. The powders were then dried at room temperature. The resulting phosphate coated CoFe was then mixed with 0.75 wt.% of the lubricant N,N' ethylene bis-stearamide (trade name: Acrawax C) and hot pressed to form a consolidated soft magnetic material referred to as CoFeP. With an avenue of synthesis for CoFeP determined, a proper amount of stock was synthesized for continuous “brick” production. While under current optimization, these 1x1 mm magnetic bricks will ultimately be placed and secured along the inside wall of each MK Magnetics transformer core by an appropriate CoFeP dispersed epoxy. As of now each brick has been produced though a pressing and annealing process via square 2x2 cm die. Before a brick is made a pressure calculation is run to ensure the dies maximum operating pressure is not exceeded. Figure 1. ensures the user’s safety by showing that the tons-on-ram required for a 2x2 cm square die to reach 760 MPa is below the point of die failure.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Compositing and Characterization of SE Quadrant Waste Exemplars

This report outlines the experimental investigation and characterization of transport properties in Hanford SE quadrant High-Level Waste (HLW). The goal of the study was to establish baseline behaviors of bulk composite rheology and settling characteristics to facilitate waste treatment process design for the Waste Treatment and Immobilization Plant (WTP) and avoid waste conditions and properties favorable to bubble cascade gas release events. The study focused on two major objectives: 1) identifying, obtaining, and preparing relevant Hanford tank waste samples for evaluation and 2) quantifying the “as-received” rheology and transport properties of the samples. Twenty-three centrifuged core segments originating from tanks AN-101, AN-106, and AW-105 were selected based on compositional relevance to SE quadrant PUREX cladding waste. These materials were composited into five waste composites enriched with target analytes: aluminum (Al), iron (Fe), phosphate (PO 4 ), uranium (U), and zirconium (Zr). Physical property and transport testing examined particle size distributions, bulk densities, settling behaviors, rheological properties, shear strengths, and just-suspended mixing speeds (NJS). Testing revealed two distinct composite classifications based on rheological characteristics: non-Newtonian composites (Fe and PO 4 ) and Newtonian composites (Al, U, and Zr). The Fe and PO 4 composites exhibited slow settling rates and reduced mobilization proclivity, attributable to strong particle-particle interactions and the formation of yield structures within non-Newtonian slurries. In contrast, the Al, U, and Zr composites displayed rapid settling and dense compaction behaviors, indicative of minimal structuring and interactions. Shear strengths for all composites were generally low relative to prior studies of SE quadrant waste, with only the U composite showing elevated strength approaching values reported in previous literature. Repeat shear strength measurements revealed contributions from dense granular material in the U composite and stronger cohesive properties in the Al composite. Settling data highlighted hindered settling behavior, with rates falling more than one order of magnitude below estimates based on Stokes’ law and rate decreasing as composite UDS content increased. NJS testing demonstrated different mobilization behaviors between cohesive and granular composites. The Fe composite required the highest mixing rate for resuspension, while the Al composite was the easiest to resuspend. Comparison of measured NJS against predictions made using the Zwietering correlation suggests non-Newtonian behavior alters resuspension mechanics, rendering non-Newtonian systems more stable against resuspension lift forces relative to their granular counterparts.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2024

Status and prospects of lithium iron phosphate manufacturing in the lithium battery industry

Abstract Lithium iron phosphate (LiFePO 4 , LFP) has long been a key player in the lithium battery industry for its exceptional stability, safety, and cost-effectiveness as a cathode material. Major car makers (e.g., Tesla, Volkswagen, Ford, Toyota) have either incorporated or are considering the use of LFP-based batteries in their latest electric vehicle (EV) models. Despite LFP’s well-researched status as a cathode material, it is expected to fulfill additional demands in electric vehicle applications, such as fast-charging capabilities, wide temperature range adaptability, and higher energy density. This perspective examines the LFP supply chain, synthetic approaches, manufacturing processes, market trends, recent advancements, and evolving demands to better understand its future role in the EV market. Graphical abstract

Lu, Yanying↗
DOE OSTI2020

A bifunctional salvage pathway for two distinct S-adenosylmethionine by-products that is widespread in bacteria, including pathogenic Escherichia coli

S-adenosyl-L-methionine (SAM) is a necessary co-substrate for numerous essential enzymatic reactions including protein and nucleotide methylations, secondary metabolite synthesis, and radical-mediated processes. Radical SAM enzymes produce 5’-deoxyadenosine, and SAM-dependent enzymes for polyamine, neurotransmitter, and quorum sensing compound synthesis produce 5’-methylthioadenosine as byproducts. Both are inhibitory and must be addressed by all cells. This work establishes a bifunctional oxygen-independent salvage pathway for 5’-deoxyadenosine and 5’-methylthioadenosine in both Rhodospirillum rubrum and Extraintestinal Pathogenic Escherichia coli. Homologous genes for this pathway are widespread in bacteria, notably pathogenic strains within several families. A phosphorylase (Rhodospirillum rubrum) or separate nucleoside and kinase (Escherichia coli) followed by an isomerase and aldolase sequentially function to salvage these two wasteful and inhibitory compounds into adenine, dihydroxyacetone phosphate and acetaldehyde or (2-methylthio)acetaldehyde during both aerobic and anaerobic growth. Both SAM byproducts are metabolized with equal affinity during aerobic and anaerobic growth conditions, suggesting that the dual-purpose salvage pathway plays a central role in numerous environments, notably the human body during infection. Finally, our newly discovered bifunctional oxygen-independent pathway, widespread in bacteria, salvages at least two byproducts of SAM-dependent enzymes for carbon and sulfur salvage, contributing to cell growth.

09 BIOMASS FUELS↗
DOE OSTI2022

13 C-metabolic flux analysis of Clostridium ljungdahlii illuminates its core metabolism under mixotrophic culture conditions

Carbon dioxide-fixing acetogenic bacteria (acetogens) utilizing the Wood-Ljungdahl Pathway (WLP) play an important role in CO 2 fixation in the biosphere and in the development of biological processes – alone or in cocultures, under both autotrophic and mixotrophic conditions – for production of chemicals and fuels. To date, limited work has been reported in experimentally validating and quantifying reaction fluxes of their core metabolic pathways. Here, the core metabolic model of the acetogen Clostridium ljungdahlii was interrogated using 13 C-metabolic flux analysis ( 13 C-MFA), which required the development of a new defined culture medium. Autotrophic, heterotrophic, and mixotrophic growth in defined medium was possible by adding 1 mM methionine to replace yeast extract. Our 13 C-MFA found an incomplete TCA cycle and inactive core pathways/reactions, notably those of the oxidative pentose phosphate pathway, Entner-Doudoroff pathway, and malate dehydrogenase. 13 C-MFA during mixotrophic growth using the parallel tracers [1– 13 C]fructose, [1,2– 13 C]fructose, [1,2,3– 13 C]fructose, and [U– 13 C]asparagine found that externally supplied CO 2 contributed the majority of carbon consumed. All internally-produced CO 2 from the catabolism of asparagine and fructose was consumed by the WLP. While glycolysis of fructose was active, it was not a major contributor to overall production of ATP, NADH, and acetyl-CoA. Gluconeogenic reactions were active despite the availability of organic carbon. Asparagine was catabolized equally via conversion to threonine and subsequent cleavage to produce acetaldehyde and glycine, and via deamination to fumarate and then the anaplerotic conversion of malate to pyruvate. Both pathways for asparagine catabolism produced acetyl-CoA, either directly via pyruvate or indirectly via the WLP. Cofactor stoichiometry based on our data predicted an essentially zero flux through the ferredoxin-dependent transhydrogenase (Nfn) reaction. Instead, nearly all of NADPH generated from the hydrogenase reaction was consumed by the WLP. Reduced ferredoxin produced by the hydrogenase reaction and glycolysis was mostly used for ATP generation via the RNF/ATPase system, with the remainder consumed by the WLP. NADH produced by RNF/ATPase was entirely consumed via the WLP.

13C metabolic flux analysis↗
DOE OSTI2022

Deciphering the Distribution and Crystal-Chemical Environment of Arsenic, Lead, Silica, Phosphorus, Tin, and Zinc in a Porous Ferrihydrite Grain Using Transmission Electron Microscopy and Atom Probe Tomography

Here the interaction of contaminants and nutrients with soil constituents is controlled by processes in intergranular and intragranular pore spaces of organic matter or/and common secondary minerals such as ferrihydrite, ~Fe 3+ 10 O 14 (OH) 2 . This contribution shows that distribution and clustering of the contaminants As, P, Pb, Si, Sn, and Zn in a porous ferrihydrite grain is greatly affected by the heterogeneous size distribution and chemical composition of the pores as well as the ability of their polyhedra to polymerize with the same type of polyhedron. Transmission electron microscopy (TEM) and atom probe tomography (APT) studies are conducted on focused ion beam (FIB) sections extracted from a porous ferrihydrite grain from the smelter-impacted topsoil in Sudbury, Ontario, Canada. The ferrihydrite grain has pore spaces ranging in diameter from tens to hundreds of nanometers. TEM and scanning-TEM studies indicate that the surfaces of the pore walls are enriched in Si. APT data in conjunction with First Near Neighbor (1NN) analyses indicate different degrees of clustering of Pb, As, Sn, Zn, Si, and P within the sample and selected domains. Careful evaluations of 3D atomic plots and 1NN distances indicates the occurrence of polymerized arsenite-, silica-, Sn-, and Zn-polyhedra within pore spaces of the ferrihydrite. Deciphering adsorption, polymerization, and nucleation processes in porous Fe-(hydr)oxides and other soil constituents requires multianalytical approaches and, in this regard, we discuss the advantages and disadvantages of the combination of TEM and APT for characterizing complex environmental samples at the atomic to nanometer scale.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗