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DOE OSTI2016

AmeriFlux US-Lin Lindcove Orange Orchard

This is the AmeriFlux version of the carbon flux data for the site US-Lin Lindcove Orange Orchard. Site Description - The experimental site was a citrus orchard about three km west of the UC Lindcove Research and Experiment Station. The site is characterized by a Mediterranean climate typical of Central California, with warm dry summers and cool wet winters. The soil texture for the upper horizon (0-33 cm) was loam with a particle size distribution of 42% sand, 38% silt, and 20% clay (Kearney Ag Center). Soil pH was 7.4 (Valley Tech Soil Agricultural Laboratory Services). The orchard was drip-irrigated with water applied twice per week in the warm season to ensure water avail- ability close to field capacity. The site was kept clean from understory vegetation and mechanical pruning operations took place twice a year to limit the size ofthe orange trees for harvesting and site maintenance. The block of trees in which the tower and instruments were located was ‘Valencia’ orange on trifoliate rootstock, with a planting date in the 1960’s. The square 4 ha block had dimensions of 200 m NeS and EeW. At the end of the study, we harvested a ‘Valencia’ citrus tree from within the study block to measure citrus leaf area index (LAI) and biomass density. The tree height was 3.7 m as measured with a telescoping pole. We measured canopy radii in the four cardinal directions to calculate a planar area (as seen from above) of 12.2 m2. The mean specific leaf area (SLA) of citrus leaves was 85.4 cm2 g-1 obtained by measuring leaf area of five groups of leaf samples with a LiCor Leaf area meter (mod. LI-3100C) followed by drying and weighing. LAI for the orchard was 3.00, derived using the SLA value and the total dry mass of leaves from the harvested tree, multiplied by the plant population of 237 plants per ha as obtained from spacing measurements and Google Maps imagery.

Fares, Silvano↗

DOE OSTI2023

AmeriFlux FLUXNET-1F US-Lin Lindcove Orange Orchard

This is the AmeriFlux Management Project (AMP) created FLUXNET-1F version of the carbon flux data for the site US-Lin Lindcove Orange Orchard. This is the FLUXNET version of the carbon flux data for the site US-Lin Lindcove Orange Orchard produced by applying the standard ONEFlux (1F) software. Site Description - The experimental site was a citrus orchard about three km west of the UC Lindcove Research and Experiment Station. The site is characterized by a Mediterranean climate typical of Central California, with warm dry summers and cool wet winters. The soil texture for the upper horizon (0-33 cm) was loam with a particle size distribution of 42% sand, 38% silt, and 20% clay (Kearney Ag Center). Soil pH was 7.4 (Valley Tech Soil Agricultural Laboratory Services). The orchard was drip-irrigated with water applied twice per week in the warm season to ensure water avail- ability close to field capacity. The site was kept clean from understory vegetation and mechanical pruning operations took place twice a year to limit the size ofthe orange trees for harvesting and site maintenance. The block of trees in which the tower and instruments were located was ‘Valencia’ orange on trifoliate rootstock, with a planting date in the 1960’s. The square 4 ha block had dimensions of 200 m NeS and EeW. At the end of the study, we harvested a ‘Valencia’ citrus tree from within the study block to measure citrus leaf area index (LAI) and biomass density. The tree height was 3.7 m as measured with a telescoping pole. We measured canopy radii in the four cardinal directions to calculate a planar area (as seen from above) of 12.2 m2. The mean specific leaf area (SLA) of citrus leaves was 85.4 cm2 g-1 obtained by measuring leaf area of five groups of leaf samples with a LiCor Leaf area meter (mod. LI-3100C) followed by drying and weighing. LAI for the orchard was 3.00, derived using the SLA value and the total dry mass of leaves from the harvested tree, multiplied by the plant population of 237 plants per ha as obtained from spacing measurements and Google Maps imagery.

Fares, Silvano↗

DOE OSTI2018

Sap flux measurements in wet tropical forests: unique challenges and opportunities

Tropical rainforests often have great tree species and functional diversity, complex age and stand structure, deep active sapwood, and potential factors that reduce transpiration, such as frequent cloud cover and wet leaves. Such factors generate challenges for estimating transpiration from sap flux measurements. In fact, upscaling approaches have rarely been attempted for diverse tropical forests. Thus, the objective of this paper is to build upon past efforts to scale transpiration and optimize strategies for wet tropical forests. Over a five-year period, we instrumented 44 trees with heat dissipation sap flow sensors within a premontane wet tropical rainforest in Costa Rica (5000 mm MAP). Given high diversity, few instrumented trees belonged to the same species, genus, or even family. In a subset of trees, radial profiles across the full range of active xylem were examined. Measurements were scaled to the stand in two plots using sapwood area. In association with extensive micrometeorological measurements, only ~10% of rainfall was transpired from this forested watershed due to persistent low radiation, evaporative demand, and frequent wet canopy conditions. Contrary to temperate trees, we observed minimal flow reductions in deeper sapwood among the largest trees, whose water use amounted to nearly 80% of the total stand water use, even though they contributed less than 15% to total stand basal area. We found that transpiration was suppressed when leaves were wet, even after accounting for lower vapor pressure deficit and reduced solar radiation. Since soil moisture conditions at this site remain continually above deficit levels, flow reversal has been assumed to be minor and thus has not yet been investigated. The driest month on record resulted in higher, not lower transpiration. Given the high diversity of these forests, herein we propose practical and innovate approaches to group trees by function or degree of canopy exposure. Finally, these efforts are critical for accurate scaling of measurements from individual sensors to stands and for improving global land surface models that increasingly partition canopy components to better represent these functionally and structurally diverse ecosystems.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2022

Guard-cell phytochromes impact seedling photomorphogenesis and rosette leaf morphology

Using a previously established transgenic approach to inactivate phytochrome chromophore synthesis in specific organs or tissues, we used a guard cell-specific promoter to induce phytochrome deficiencies in guard cells of Arabidopsis thaliana. Analyses of multiple homozygous lines depleted of phytochromes in stomatal guard cells indicated elongated hypocotyls specifically in red and far-red growth conditions. Furthermore, rosette leaves of adult plants with guard cell-specific phytochrome deficiencies showed enhanced serration compared to the wild-type Col-0 parent. Thus, we demonstrate that guard cell-localized phytochromes impact the inhibition of hypocotyl elongation, as well as leaf margin morphology of adult rosette leaves in A. thaliana.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2011

Evaluation of the residue from microset on various metal surfaces.

Fast-curing impression materials are sometimes used to cast negative-mold replications of physical defects on material surfaces. The negative-mold impressions can then be used for further measurements to record the nature of the defect. These impression materials have been designed to cure quickly, and with very low adhesion, so that they can be easily removed from the surface leaving little residual contamination. Unfortunately, some contaminant is retained by the substrate material. This investigation seeks to identify the composition and quantity of the remaining material upon removal of Microset Synthetic Rubber Replicating Compound from several material surfaces. Coe-Flex was used as a relative comparison to Microset. On fifteen different substrate materials the Microset leaves no visible trace of contaminant, however, X-ray photoelectron spectroscopy shows evidence of a thin silicone-based contaminant film of approximately 2 nm thickness.

36 MATERIALS SCIENCE↗

DOE OSTI2012

Treatability Study for Edible Oil Deployment for Enhanced cVOC Attenuation for T-Area, Savannah River Site

Groundwater beneath T-Area, a former laboratory and semiworks operation at the Department of Energy (DOE) Savannah River Site (SRS), is contaminated by chlorinated solvents (cVOCs). Since the contamination was detected in the 1980s, the cVOCs at T-Area have been treated by a combination of soil vapor extraction and groundwater pump and treat. The site received approval to temporarily discontinue the active groundwater treatment and implement a treatability study of enhanced attenuation - an engineering and regulatory strategy that has recently been developed by DOE and the Interstate Technology and Regulatory Council (ITRC 2007). Enhanced attenuation uses active engineering solutions to alter the target site in such a way that the contaminant plume will passively stabilize and shrink and to document that the action will be effective, timely, and sustainable. The paradigm recognizes that attenuation remedies are fundamentally based on a mass balance. Thus, long-term plume dynamics can be altered either by reducing the contaminant loading from the source or by increasing the rate of natural attenuation processes within all, or part of, the plume volume. The combination of technologies that emerged for T-Area included: (1) neat (pure) vegetable oil deployment in the deep vadose zone in the former source area, (2) emulsified vegetable oil deployment within the footprint of the groundwater plume, and (3) identification of attenuation mechanisms and rates for the distal portion of the plume. In the first part, neat oil spreads laterally forming a thin layer on the water table to intercept and reduce future cVOC loading (via partitioning) and reduce oxygen inputs (via biostimulation). In the second and third parts, emulsified oil forms active bioremediation reactor zones within the plume footprint to degrade existing groundwater contamination (via reductive dechlorination and/or cometabolism) and stimulates long-term attenuation capacity in the distal plume (via cometabolism). For TArea, the enhanced attenuation development process proved to be a powerful tool in developing a strategy that provides a high degree of performance while minimizing adverse collateral impacts of the remediation (e.g., energy use and wetland damage) and minimizing life-cycle costs. As depicted in Figure 1, Edible oil deployment results in the development of structured geochemical zones and serves to decrease chlorinated compound concentrations in two ways: (1) physical sequestration, which reduces effective aqueous concentration and mobility; and (2) stimulation of anaerobic, abiotic and cometabolic degradation processes. In the central deployment area, contaminant initially partitions into the added oil phase. Biodegradation of the added organic substrate depletes the aquifer of oxygen and other terminal electron acceptors and creates conditions conducive to anaerobic degradation processes. The organic substrate is fermented to produce hydrogen, which is used as an electron donor for anaerobic dechlorination by organisms such as Dehalococcoides. Daughter products leaving the central treatment zone are amenable to aerobic oxidation. Further, the organic compounds leaving the central deployment zone (e.g., methane and propane) stimulate and enhance down gradient aerobic cometabolism which degrades both daughter compounds and several parent cVOCs. Figure 1 depicts TCE concentration reduction processes (labeled in green) along with their corresponding breakdown products in a structured geochemical zone scenario. A consortium of bacteria with the same net effect of Dehalococcoides may be present in the structured geochemical zones leading to the degradation of TCE and daughter products. Figure 2 shows a schematic of the documented cVOC degradation processes in both the anaerobic and aerobic structured geochemical zones. Specific aerobic and anaerobic bacteria and their degradation pathways are also listed in the diagram and have either been confirmed in the field or the laboratory. See references in the bibliography in Section 11.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2012

Development of high-spatial and high-mass resolution mass spectrometric imaging (MSI) and its application to the study of small metabolites and endogenous molecules of plants

High-spatial and high-mass resolution laser desorption ionization (LDI) mass spectrometric (MS) imaging technology was developed for the attainment of MS images of higher quality containing more information on the relevant cellular and molecular biology in unprecedented depth. The distribution of plant metabolites is asymmetric throughout the cells and tissues, and therefore the increase in the spatial resolution was pursued to reveal the localization of plant metabolites at the cellular level by MS imaging. For achieving high-spatial resolution, the laser beam size was reduced by utilizing an optical fiber with small core diameter (25 μm) in a vacuum matrix-assisted laser desorption ionization-linear ion trap (vMALDI-LTQ) mass spectrometer. Matrix application was greatly improved using oscillating capillary nebulizer. As a result, single cell level spatial resolution of ~ 12 μm was achieved. MS imaging at this high spatial resolution was directly applied to a whole Arabidopsis flower and the substructures of an anther and single pollen grains at the stigma and anther were successfully visualized. MS imaging of high spatial resolution was also demonstrated to the secondary roots of Arabidopsis thaliana and a high degree of localization of detected metabolites was successfully unveiled. This was the first MS imaging on the root for molecular species. MS imaging with high mass resolution was also achieved by utilizing the LTQ-Orbitrap mass spectrometer for the direct identification of the surface metabolites on the Arabidopsis stem and root and differentiation of isobaric ions having the same nominal mass with no need of tandem mass spectrometry (MS/MS). MS imaging at high-spatial and high-mass resolution was also applied to cer1 mutant of the model system Arabidopsis thaliana to demonstrate its usefulness in biological studies and reveal associated metabolite changes in terms of spatial distribution and/or abundances compared to those of wild-type. The spatial distribution of targeted metabolites, mainly waxes and flavonoids, was systematically explored on various organs, including flowers, leaves, stems, and roots at high spatial resolution of ~ 12-50 μm and the changes in the abundance level of these metabolites were monitored on the cer1 mutant with respect to the wild-type. This study revealed the metabolic biology of CER1 gene on each individual organ level with very detailed high spatial resolution. The separate MS images of isobaric metabolites, i.e. C29 alkane vs. C28 aldehyde could be constructed on both genotypes from MS imaging at high mass resolution. This allows tracking of abundance changes for those compounds along with the genetic mutation, which is not achievable with low mass resolution mass spectrometry. This study supported previous hypothesis of molecular function of CER1 gene as aldehyde decarbonylase, especially by displaying hyper accumulation of aldehydes and C30 fatty acid and decrease in abundance of alkanes and ketones in several plant organs of cer1 mutant. The scope of analytes was further directed toward internal cell metabolites from the surface metabolites of the plant. MS profiling and imaging of internal cell metabolites were performed on the vibratome section of Arabidopsis leaf. Vibratome sectioning of the leaf was first conducted to remove the surface cuticle layer and it was followed by enzymatic treatment of the section to induce the digestion of primary cell walls, middle lamella, and expose the internal cells underneath to the surface for detection with the laser by LDI-MS. The subsequent MS imaging onto the enzymatically treated vibratome section allowed us to map the distribution of the metabolites in the internal cell layers, linolenic acid (C18:3 FA) and linoleic acid (C18:2 FA). The development of an assay for relative quantification of analytes at the single subcellular/organelle level by LDI-MS imaging was attempted and both plausibility and significant obstacles were seen. As a test system, native plant organelle, chloroplasts isolated from the spinach leaves were used and the localization of isolated chloroplasts dispersed on the target plate in low density was monitored by detecting the ion signal of chlorophyll a (Chl a) degradation products such as pheophytin a and pheophobide a by LDI-MS imaging in combination with fluorescence microscopy. The number of chloroplasts and their localization visualized in the MS image exactly matched those in the fluorescence image especially at low density, which first shows the plausibility of single-organelle level quantification of analytes by LDI-MS. The accumulation level of Chl a within a single chloroplast detected by LDI-MS was compared to the fluorescence signal on a pixel-to-pixel basis to further confirm the correlations of the accumulation levels measured by two methods. The proportional correlation was observed only for the chloroplasts which do not show the significant leakage of chlorophyll indicated by MS ion signal of Chl a degradation products and fluorescence signal, which was presumably caused by the prior fluorescence measurement before MS imaging. Further investigation is necessary to make this method more complete and develop LDI-MS imaging as an effective analytical tool to evaluate a relative accumulation of analytes of interest at the single subcellular/organelle level.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2012

Sulfur Hexafluoride Treatment of Used Nuclear Fuel to Enhance Separations

Reactive Gas Recycling (RGR) technology development has been initiated at Savannah River National Laboratory (SRNL), with a stretch-goal to develop a fully dry recycling technology for Used Nuclear Fuel (UNF). This approach is attractive due to the potential of targeted gas-phase treatment steps to reduce footprint and secondary waste volumes associated with separations relying primarily on traditional technologies, so long as the fluorinators employed in the reaction are recycled for use in the reactors or are optimized for conversion of fluorinator reactant. The developed fluorination via SF 6 , similar to the case for other fluorinators such as NF 3 , can be used to address multiple fuel forms and downstream cycles including continued processing for LWR via fluorination or incorporation into a aqueous process (e.g. modified FLUOREX) or for subsequent pyro treatment to be used in advanced gas reactor designs such metal- or gas-cooled reactors. This report details the most recent experimental results on the reaction of SF 6 with various fission product surrogate materials in the form of oxides and metals, including uranium oxides using a high-temperature DTA apparatus capable of temperatures in excess of 1000°C. The experimental results indicate that the majority of the fission products form stable solid fluorides and sulfides, while a subset of the fission products form volatile fluorides such as molybdenum fluoride and niobium fluoride, as predicted thermodynamically. Additional kinetic analysis has been performed on additional fission products. A key result is the verification that SF 6 requires high temperatures for direct fluorination and subsequent volatilization of uranium oxides to UF 6 , and thus is well positioned as a head-end treatment for other separations technologies, such as the volatilization of uranium oxide by NF 3 as reported by colleagues at PNNL, advanced pyrochemical separations or traditional full recycle approaches. Based on current results of the research at SRNL on SF 6 fluoride volatility for UNF separations, SF 6 treatment renders all anticipated volatile fluorides studied to be volatile, and all non-volatile fluorides studied to be non-volatile, with the notable exception of uranium oxides. This offers an excellent opportunity to use this as a head-end separations treatment process because: 1. SF 6 can be used to remove volatile fluorides from a UNF matrix while leaving behind uranium oxides. Therefore an agent such as NF 3 should be able to very cleanly separate a pure UF 6 stream, leaving compounds in the bottoms such as PuF 4 , SrF 2 and CsF after the UNF matrix has been pre-treated with SF 6 . 2. Due to the fact that the uranium oxide is not separated in the volatilization step upon direct contact with SF 6 at moderately high temperatures (≤ 1000°C), this fluoride approach may be well-suited for head-end processing for Gen IV reactor designs where the LWR is treated as a fuel stock, and it is not desired to separate the uranium from plutonium, but it is desired to separate many of the volatile fission products. 3. It is likely that removal of the volatile fission products from the uranium oxide should simplify both traditional and next generation pyroprocessing techniques. 4. SF 6 treatment to remove volatile fission products, with or without treatment with additional fluorinators, could be used to simplify the separations of traditional aqueous processes in similar fashion to the FLUOREX process. Further research should be conducted to determine the separations efficiency of a combined SF 6 /NF 3 separations approach which could be used as a stand-alone separations technology or a head-end process.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2012

Post-Retrofit Residential Assessments

This study examined a range of factors influencing energy consumption in households that had participated in residential energy-efficiency upgrades. The study was funded by a grant from the U.S. Department of Energy’s Pacific Northwest National Laboratory and was conducted by faculty and staff of Portland State University Center for Urban Studies and Department of Economics. This work was made possible through the assistance and support of the Energy Trust of Oregon (ETO), whose residential energy-efficiency programs provided the population from which the sample cases were drawn. All households in the study had participated in the ETO Home Performance with Energy Star (HPwES) program. A number of these had concurrently pursued measures through other ETO programs. Post-retrofit energy outcomes are rarely investigated on a house-by-house basis. Rather, aggregate changes are ordinarily the focus of program impact evaluations, with deviation from aggregate expectations chalked up to measurement error, the vagaries of weather and idiosyncrasies of occupants. However, understanding how homes perform post-retrofit on an individual basis can give important insights to increase energy savings at the participant and the programmatic level. Taking a more disaggregated approach, this study analyzed energy consumption data from before and after the retrofit activity and made comparisons with engineering estimates for the upgrades, to identify households that performed differently from what may have been expected based on the estimates. A statistical analysis using hierarchal linear models, which accounted for weather variations, was performed looking separately at gas and electrical use during the periods before and after upgrades took place. A more straightforward comparison of billing data for 12-month periods before and after the intervention was also performed, yielding the majority of the cases examined. The later approach allowed total energy use and costs to be assessed but did not account for weather variation. From this statistical analysis, 18 study participants were selected and interviewed. The participants completed an in-home interview covering a range of topics, including changes in occupancy and additional changes to the homes that may have affected energy use. The goal of the interviews was to identify factors that may have contributed to unusual energy performance. These factors were identified by their frequency of occurrence in outperforming or underperforming homes, or simply by identifying factors that had the largest impact on overall savings. The motivations and levels of satisfaction with the outcomes of the upgrades were covered in detail, as well as extensive discussions of behaviors pertaining to thermal control, lighting, water, and appliance use. Most of cases studied achieved substantial energy savings, although it was more common for the projected savings to be greater than the demonstrated savings. Two factors that played a very large role in savings variation were 1) changes in occupancy and 2) fenestration improvements outside of the incentive programs. Motivation for pursuing the upgrades (e.g., environmental sustainability vs. comfort or cost savings) did not seem to play any role in achieving savings. Participants generally were more concerned with maintaining aesthetics through lighting than comfort through heating or cooling. They also seemed more likely to turn the lights off when leaving a room than to turn the heat off when leaving the home.

high performance homes↗

DOE OSTI2013

New Synthetic Methods and Structure-Property Relationships in Neptunium, Plutonium, and Americium Borates. Final report

The past three years of support by the Heavy Elements Chemistry Program have been highly productive in terms of advanced degrees awarded, currently supported graduate students, peer-reviewed publications, and presentations made at universities, national laboratories, and at international conferences. Ph.D. degrees were granted to Shuao Wang and Juan Diwu, who both went on to post-doctoral appointments at the Glenn T. Seaborg Center at Lawrence Berkeley National Laboratory with Jeff Long and Ken Raymond, respectively. Pius Adelani completed his Ph.D. with me and is now a post-doc with Peter C. Burns. Andrea Alsobrook finished her Ph.D. and is now a post-doc at Savannah River with Dave Hobbs. Anna Nelson completed her Ph.D. and is now a post-doc with Rod Ewing at the University of Michigan. As can be gleaned from this list, students supported by the Heavy Elements Chemistry grant have remained interested in actinide science after leaving my program. This follows in line with previous graduates in this program such as Richard E. Sykora, who did his post-doctoral work at Oak Ridge National Laboratory with R. G. Haire, and Amanda C. Bean, who is a staff scientist at Los Alamos National Laboratory, and Philip M. Almond and Thomas C. Shehee, who are both staff scientists at Savannah River National Laboratory, Gengbang Jin who is a staff scientist at Argonne National Lab, and Travis Bray who has been a post-doc at both LBNL and ANL. Clearly this program is serving as a pipe-line for students to enter into careers in the national laboratories. About half of my students depart the DOE complex for academia or industry. My undergraduate researchers also remain active in actinide chemistry after leaving my group. Dan Wells was a productive undergraduate of mine, and went on to pursue a Ph.D. on uranium and neptunium chalcogenides with Jim Ibers at Northwestern. After earning his Ph.D., he went directly into the nuclear industry.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2014

Samuel P. Massie Chair of Excellence In Environmental Disciplines: Hampton University 1994-2010 Year Report

The establishment of the DOE-EM Dr. Samuel P. Massie Chair of Excellence provides an excellent opportunity for Hampton University to be involved in key environmental issues in the 21 st Century. The main areas of focus are on: 1. Coal gasification with respect to pollution prevention and reduction. 2. Solid waste treatment through bioremediation technology and 3. Industrial wastewater treatment Synthesizing ion catalysts suitable for use in slurry bubble column reaction was carried out. Construction of an autoclave continuous stirred tank reactor has been completed. At the initial stage of the development of this program, work was conducted in the area of formic acid recovery from waste streams, which yielded useful results. We also succeeded in the removal of priority metal ions such as cadmium, chromium, copper, lead, mercury, nickel, silver, thallium, zinc, etc., from industrial and municipal wastewater by using natural wastes. The process uses tree leaves to adsorb the metal ions in the wastewater. The ultimate goal is to develop inexpensive, highly available, effective metal ion adsorbents from natural wastes as an alternative to existing commercial adsorbents, and also to explain the possible adsorption mechanism that is taking place. This technology uses natural wastes to eliminate other wastes. Obviously, there are several advantages: (1) the negative impact on environment is eliminated, (2) the complicated regeneration step is not needed, and (3) the procedure saves money and energy. Twelve different types of leaves have been tested with lead, zinc, and nickel. The study mechanism showed that the leaf tannin is an active ingredient in the adsorption of metal ions. The ion-exchange mechanism controlled the adsorption process.

42 ENGINEERING↗

DOE OSTI2014

Quantity of 135 I released from the AGR-1, AGR-2, and AGR-3/4 experiments and discovery of 131 I at the FPMS traps during the AGR-3/4 experiment

A series of three Advanced Gas Reactor (AGR) experiments have been conducted in the Advanced Test Reactor (ATR) at Idaho National Laboratory (INL). From 2006 through 2014, these experiments supported the development and qualification of the new U.S. tristructural isotropic (TRISO) particle fuel for Very High Temperature Reactors (VHTR). Each AGR experiment consisted of multiple fueled capsules, each plumbed for independent temperature control using a mix of helium and neon gases. The gas leaving a capsule was routed to individual Fission Product Monitor (FPM) detectors. For intact fuel particles, the TRISO particle coatings provide a substantial barrier to fission product release. However, particles with failed coatings, whether because of a minute percentage of initially defective particles, those which fail during irradiation, or those designed to fail (DTF) particles, can release fission products to the flowing gas stream. Because reactive fission product elements like iodine and cesium quickly deposit on cooler capsule components and piping structures as the effluent gas leaves the reactor core, only the noble fission gas isotopes of Kr and Xe tend to reach FPM detectors. The FPM system utilizes High Purity Germanium (HPGe) detectors coupled with a thallium activated sodium iodide NaI(Tl) scintillator. The HPGe detector provides individual isotopic information, while the NaI(Tl) scintillator is used as a gross count rate meter. During irradiation, the 135m Xe concentration reaching the FPM detectors is from both direct fission and by decay of the accumulated 135 I. About 2.5 hours after irradiation (ten 15.3 minute 135m Xe half lives) the directly produced 135m Xe has decayed and only the longer lived 135 I remains as a source. Decay systematics dictate that 135m Xe will be in secular equilibrium with its 135 I parent, such that its production rate very nearly equals the decay rate of the parent, and its concentration in the flowing gas stream will appear to decay with the parent half life. This equilibrium condition enables the determination of the amount of 135 I released from the fuel particles by measurement of the 135m Xe at the FPM following reactor shutdown. In this paper, the 135 I released will be reported and compared to similar releases for noble gases as well as the unexpected finding of 131 I deposition from intentional impure gas injection into capsule 11 of experiment AGR 3/4.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2015

A Compact, Broad-Band Hyperspectral SpectroRadiometer (Final Report)

The Phase I effort has laid the foundation for developing a complete, high-performance hyperspectral imaging system based on a patented approach. Detailed optical modeling has been performed to identify an optimal design that promises excellent imaging, low stray-light, and large signal-to-noise ratios across the full spectral range of 350-2500 nm. Vibration analysis indicates the instrument’s primary optics will be stable when deployed in high-vibration environments such as onboard a UAV, and a mechanical design has been developed. A two-step development plan has been formulated to minimize risk. In the first step, a deployable prototype instrument will be built that provides full performance but will utilize a somewhat heavy, but proven, data acquisition system. This will leave sufficient time and resources to address problems that may arise and incorporate a more advanced data acquisition system during the second step, plus leave time and resources to make other improvements identified during testing done during the first step. In summary, the effort will lead to an advanced instrument for vegetation monitoring, which may find applications in agriculture, pipeline monitoring, and it will find applications for a broad range of research including work devoted to understanding of the carbon cycle.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2017

The dual effect of tubulin manipulation on Populus wood formation and drought tolerance

The main objectives were to generate transgenic Populus with altered alpha- (TUA) and beta-tubulin (TUB) expression and/or post-translational modifications (PTMs) in a plant-wide, guard cell-specific or xylem-specific manner, and then to characterize the effects of the modifications on tree growth and wood properties. In short, strong effects on cell wall composition were noted in leaves where transgene expression was strong (Harding et al. 2017; Hu et al. in review). Subtle, but noteworthy effects were observed in wood (developing xylem) where transgene expression was weak (Swamy et al. 2015). Any effect of PTM manipulation was functionally recessive and/or confounded by tubulin overexpression. It was anticipated that PTM manipulation would affect tubulin half-life, and this is the question that was being addressed, but overall tubulin protein levels correlated with transgene expression levels. We also demonstrated that a dynamic C-terminal PTM known as the tyrosination/detyrosination cycle, so common in animal systems, and purportedly operational in plants, does not occur in wood-forming tissues of Populus (Hu et al. 2016). Contrary to the commonly hypothesized role of microtubules in directing microfibril deposition, cellulose content and microfibril angle were not changed in tubulin-overexpressing plants, nor were hemicellulose and lignin contents, in either wood or leaves. Instead, this project demonstrated that the extractability of pectin and xylan polysaccharides was sensitive to tubulin perturbations, with consequences in stomatal stress response and lignocellulosic biomass utilization. The work also revealed a complex interplay by multi-compartmental (cell wall and cytoskeleton) signaling that impinged upon the control of phenylpropanoid metabolic flux to modulate stomatal response to environmental stimuli.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2019

Broad Scope Analysis of the MOX Fuel Fabrication Facility and Disposition of Plutonium

The Plutonium Management and Disposition Agreement (PMDA), signed into effect in 2000, between the United States and Russia, was made in a post-Cold War effort to dispose of military-useable material, a combined 68 metric tons of weapon-grade plutonium. The United States has been pursuing a disposition path through conversion to MOX fuel for use in current commercial nuclear reactors. The Savannah River Site’s (SRS) MOX Fuel Fabrication Facility (MFFF, the MOX facility) began construction in 2007 with intent to uphold the United States’ half of the agreement. In the FY2017 budget, the Obama administration proposed a termination of the MFFF after lack of sufficient funding to the project, which caused paralyzing delays and drastically inflated costs for completion. Prolonged construction, piled costs, and divergent policies between shifting administrations have resulted in turmoil between the United States and Russia, culminating with the proposed abandonment of the MOX disposition path and being used as a justification by Russia to withdraw from the agreement until the United States is able to identify a clear plan, fulfilling the requirements set forth by the PMDA. The leading expedient to replace MOX fuel is the dilute and dispose method, which leaves uncertainty for the SRS MFFF and places reliance on New Mexico’s Waste Isolation Pilot Plant (WIPP) to legally accommodate the additional and unaccounted waste. If the current capacity of WIPP proves insufficient, construction of a new repository for transuranic waste would only incur additional costs and regulatory burdens, along with extreme schedule delays. Future proposed adaptations of the SRS MFFF include pit production, which would require complex and costly alterations to be operational at the current site. Restrictions from Congress, such as mandating the proposed solution to abandoning MFFF must equal half of the costs required for completing the facility, have fueled severely underestimated quotations of these alternatives. The increasing pressure from both Russia and South Carolina government officials to make a decision could result in the pursuit of another doomed project, leaving the United States with even further sunk costs and strained international relations. This paper will summarize the involved history of the MFFF, explicate the recourses to salvage the facility for pit production, and provide postulation on the dilute and dispose method.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2019

Energy Storage Financing: Advancing Contracting in Energy Storage

The lack of standard financing contracts and supporting documents is inhibiting the growth of the energy storage industry. A number of firms are actively developing proprietary contract structures, resulting in a variety of unique attributes. This leaves the market disjointed for 3 rd party financing groups looking to scale their lending. Lack of commonality and harmonization between developer and lenders raises project execution costs and causes delays in financing. Of special concern, projects based on emerging technologies are finding an increasing uphill climb for equal consideration by developers and lenders, leaving their potential commercialization in peril. This study will evaluate the development of standardi7ed contracts to reduce the cost and contract approval time, learning from success in renewable energy project development. The goal of this study is to determine the key requirements for standard contracts in the emerging energy storage market, and suggest avenues for possible industry led development.

25 ENERGY STORAGE↗

DOE OSTI2021

Imaging Electrons in Two Dimensional Materials (Final report)

Two-dimensional (2D) materials have extraordinary characteristics that offer promising new approaches for science and technology. Electrons in graphene can move ballistically through a sheet, even though it is only a single atom thick. And transition metal dichalcogenide materials can be cleaved into 2D flakes of all types – metals, semiconductors, insulators, magnetic materials, and superconductors. To benefit from these discoveries, the science needs to be understood to transform 2D materials into useful new devices and systems. The evolution in time of atomic scale graphene structures has been studied in time with a transmission electron microscope (TEM), and ballistic transport of electrons in graphene was been imaged using a cooled scanning probe microscope (SPM), as well as electron motion in MoS 2 . Graphene is only one atom thick but is extremely strong, creating the opportunity to fabricate atomic scale structures in the lateral direction. Using an atomic resolution TEM, a suspended sheet of graphene can be shaped by a Si impurity atom on its surface that acts like a chisel to open up apertures, one atom at a time. The electrons in the TEM provide both the chiseling energy and the ability to image the results. Electrons and holes in graphene form a new type of electronic system with conical conduction and valence bands that meet at the Dirac point, with no energy gap. For moderate densities, the carriers form a Fermi liquid with ballistic transport over micron-scale distances. Using a cooled SPM the cyclotron orbit of electrons in graphene has been imaged. In the magnetic focusing regime, electrons leaving a point contact circle around and leave from a second point contact when the cyclotron diameter is equal to the contact spacing. The paths of electrons are focused - they enter at different angles but converge again at the exiting contact. When the SPM tip knocks an electron out of its orbit, an imaging signal is created. The ballistic motion of carriers in graphene opens the way for ballistic devices that manipulate beams of electrons and holes. Our collaborator Gil-Ho Lee, in Philip Kim's group, created a collimating contact by placing zig-zag absorbers on either side of entering electrons. Our cooled SPM was used to image the electron beam and determine its 9-degree halfwidth. By changing the gate voltage, a collimated beam of holes was also created, opening the way for colliding beam experiments. Coherent beams of carriers are desirable for quantum information processing. Via Andreev reflection, superconducting contacts can covert Cooper pairs in a superconductor to an ingoing and outgoing electrons and holes. Using our cooled SPM, Andreev reflection was imaged from a superconducting contact on a graphene device. Magnetic focusing was used to create an incoming beam of electrons and an outgoing beam of holes, detected by a third point contact. The images show a clear transition from normal reflection above the superconducting transition temperature to Andreev reflection as the device is cooled. Transition metal dichalcogenides offer a wide array of materials that can be exfoliated into ultrathin 2D sheets. A cooled SPM can be used to detect quantum dots as well as to image electron flow. The tip charge capacitively couples to electrons on the dot, acting as a gate to tune the dot conductance. Coulomb blockade peaks appear as a bullseye pattern in an SPM image as the tip is raster scanned above the dot. This approach was used to detect quantum dots in a MoS 2 channel as the carrier density was reduced and electrons pooled in low energy points. Through our DOE supported research, cooled SPM imaging has proven to be a very useful tool to uncover the motion of electrons and holes in the new quantum materials graphene and MoS 2 .

36 MATERIALS SCIENCE↗

DOE OSTI2023

Sticky roots--implications of widespread, cryptic, viral infection of plants in natural and managed ecosystems for soil carbon processing in the rhizosphere

Plants strongly influence soil properties through rhizodeposition, in which exudates diffuse from roots, additional secretions are actively released, and root cells are sloughed into the soil. This contribution by plants of carbon compounds belowground is at the core of soil health, water holding capacity, and the soil carbon storage that pulls carbon dioxide out of the atmosphere. Once in soil, organic matter can bind with minerals such as iron hydroxides, where it can be protected from microbial attack for millenia, preserving very large terrestrial soil carbon pools. However, those same compounds contributed by roots to soil may also destabilize the long-term protective associations of SOM with minerals, making that soil organic matter (SOM) more vulnerable to microbial attack and decomposition. Plant roots thus influence both the buildup and breakdown of soil carbon pools. DOE’s E3SM Land Model (ELM) includes a representation of soil carbon storage on minerals, but the potential vulnerability of SOM–mineral associations to effects of rhizodeposition is not yet represented in ELM. To begin testing for this effect of rhizodeposition on soil carbon storage and decomposition, we worked to develop a novel approach during this TES Exploratory project DE-SC0019142 – we harnessed the power of plant viral infection. We examined whether plant virus infection can serve as a tool to intensify rhizodeposition at the root surface, and therefore possibly intensify mobilization of SOM from minerals making it visible to our analytical techniques. Viral infection is widespread in terrestrial ecosystems; 25-70% of plants have virus infection, yet the influence of such infection on root traits and terrestrial soil carbon dynamics remains largely unexplored. We used two plant hosts: the annual Avena sativa (oats) and the genetically tractable, model grass Brachypodium distachyon. These grasses were infected with the broad host range virus Barley Yellow Dwarf Virus (BYDV) via aphids (Rhopalosiphum padi). BYDV infects at least 150 grass species in agricultural and natural ecosystems, and in previous experiments, oats infected with BYDV had roots that were very sticky to the touch, strongly suggesting that infection altered rhizodeposition. We developed this new experimental approach mostly in a one virus (Barley Yellow Dwarf Virus)–one plant (Avena sativa) system. (Several effects of infection in a Brachypodium-BYDV system were similar in nature to effects on Avena sativa, but were more variable.) In the BYDV-Avena system, we developed protocols for consistently infecting target plants (and avoiding infection of control plants) using aphid caging on leaves. We measured that infected plants exhibited reduced photosynthesis, plant (including root) biomass, and root:shoot ratio, as well as simplified root system architecture. We established procedures for sampling the organic compounds carried specifically in phloem (vascular tissue) of leaves and roots, using aphid stylectomy. We used FTICR-MS, Orbitrap GC-MS, and LC-MS/MS to analyze organic compounds in phloem, liquid around roots of plants grown hydroponically, and pore water around roots in soil, and found differences in the compounds in solution bathing roots when infected and uninfected plants were grown hydroponically. Finally, we synthesized isotopically-labeled mineral–organic matter (MAOM) associations in the lab and developed assays using them in solution and in soil. Assays quantified the extent and rate of mineralization of labeled MAOM that was mobilized by functionally distinct rhizodeposits and then attacked by microbes. Two mechanisms for MAOM mobilization emerged, with distinct dynamics. During “direct” mobilization, rhizodeposits such as the strong ligand oxalic acid could drive rapid dissolution of minerals, mobilizing MAOM. During “indirect” mobilization, rhizodeposits such as the simple sugar glucose did not attack minerals directly but instead intensified microbial activity, which led to mobilization via changes in e.g. pH, Eh, and microbial metabolite production (Li et al. 2021). Mechanistic understanding derived from these data and our ongoing experiments using these techniques will inform future development of ELM. Plant roots not only contribute newly fixed organic compounds to soils, but also root activities can drive mineralization of the carbon and nutrients mobilized off minerals via “indirect” or “direct” mechanisms. Using viral infection as a new tool, ongoing combined experimentation and modeling will explore the strength and larger-scale significance of the cascade of processes from rhizodeposition to MAOM mobilization for soil carbon storage and nutrient cycling in terrestrial ecosystems. And if viral infection leads quite generally to “sticky roots”, our perception of the potential importance of prevalent virus infection in terrestrial landscapes will be transformed.

54 ENVIRONMENTAL SCIENCES↗