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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records

Application of a headspace GC–MS method to evaluate the product quality of alcohol‐based hand wipe sanitizers

Abstract The investigation of marketed hand wipe sanitizers presented an analytical challenge owing to the need for extraction from the solid matrix of the products. The present work describes the development of a new sample preparation method for the extraction of analytes from the hand wipe sanitizer matrix into dimethyl sulfoxide for analysis using headspace GCMS. Alcohol‐based hand sanitizer (ABHS) wipe products labeled to contain ethanol or isopropanol as active ingredients were tested, varying in the size and weight of the wipes. The spike recovery assay was confirmed using spiking solutions containing impurities at concentrations equivalent to 50, 100 and 200% of the interim concentration limits. All of the tested analytes showed recovery within the allowable limits (80–120%). Six marketed ABHS wipe products were tested and no impurities above the FDA interim limits were observed. One product contained ethanol below the 60% v/v limit and another product was mislabeled for isopropanol and was found to contain ethanol instead. Four of the six ABHS products did not meet the label claim, which may affect the product quality. The analytical method and sample preparation procedures will provide the FDA and ABHS manufacturers with the capability to conduct quality assurance testing of hand wipe sanitizers for active ingredient content and impurities.

Biochemistry & Molecular Biology↗

Comparing and contrasting In-Vial and full-scale systems for sparging volatile analytes

Here, in-vial sparging was demonstrated as an effective, practical alternative to a full-scale sparging system for supporting the analysis of volatile constituents. Using elemental mercury (Hg 0 ) and toluene as representative purgeable analytes, the mass removal for various sparge configurations was measured and a reduced order model was developed and validated. In the primary experiments, Hg 0 in the sparge gas was trapped on activated carbon or gold, thermally desorbed, and quantified using atomic absorption or atomic fluorescence spectroscopy. Toluene experiments using the same in-vial sparge apparatus and sparge parameters were performed to demonstrate the applicability of the reduced order model to a broad range of compounds. Toluene removal was tracked by measuring the remaining toluene in sparged aliquots using Ultraviolet-visible (UV–Vis) spectroscopy. For the sparging, flow rates varied from 25 to 75 mL/min for periods from 0 to 30 min. Sparge performance, mass removal as a function of time, and sparge gas volume were measured for both in-vial and full-scale systems. A model based on dimensionless Henry's Law coefficient, normalized sparge gas volume, and fractional extent of equilibrium matched the experimental data for both compounds and provides a practical tool for future applications. For the conditions tested in this study, the calibrated model indicated that the sparge gas in the in-vial system reached approximately 33% of its equilibrium value before exiting the water surface, while a full-scale system reached approximately 100%. The tests validated the quality, reproducibility, and predictability of sparging performance for both full scale and in-vial sparge systems. Related factors such as waste generation, worker risk, and labor were also assessed. Full scale sparge systems provide the advantage of lower detection levels due to larger sample volume, while the in-vial sparge systems provide advantages for most other factors; including automatability, reducing secondary wastes, lessening the need to clean and check the sparge apparatus, and lowering labor and costs. The data and associated reduced order model support continued development and deployment of in-vial sparge platforms as a practical option for analysis of purgeable analytes such as volatile organic compounds and volatile metals/organometallics.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A device for volatile organic compound (VOC) analysis from skin using heated dynamic headspace sampling

Abstract Human skin is an important source of volatile organic compounds (VOCs) offering noninvasive methods to gain clinical metabolite information. This work was focused on the development of a skin sampling device based on a dynamic headspace sampling method with the addition of temperature to increase VOC metabolite recovery. The device preconcentrates skin VOC emissions onto a sorbent substrate, which can either be preserved for offline analysis or attached to a real time sensor downstream. In this work, skin VOC samples were analyzed offline using thermal desorption-gas chromatography-mass spectrometry. A list of 10 common skin VOCs was pre-selected to optimize parameters of sampling time, sampling temperature, and sorbent selection. Overall, this study highlights an effective skin VOC sampling technology with a heating dimension (40 °C, rather than 30 °C or no heating) with a sampling time of 15 min (rather than 5 or 30 mins) and onto Tenax TA sorbent (rather than PDMS), which collectively increases the recovery of compounds with lower vapor pressure and decreases the observed variability in skin VOC measurements. Finally, a list of 79 skin VOC compounds were detected and identified within a cohort of 20 young, healthy volunteers.

Biochemistry & Molecular Biology↗

Comparing the extraction performance of cyclodextrin-containing supramolecular deep eutectic solvents versus conventional deep eutectic solvents by headspace single drop microextraction

A headspace single drop microextraction (HS-SDME) method coupled with high performance liquid chromatography was developed to compare the extraction of eighteen aromatic organic pollutants from aqueous solutions using cyclodextrin-based supramolecular deep eutectic solvents (SUPRADESs) and alkylammonium halide-based conventional deep eutectic solvents (DESs). Different derivatives of beta-cyclodextrin (β-CD) were employed as hydrogen bond acceptors (HBA) in SUPRADESs and the extraction performance investigated. SUPRADES comprised of the 20 wt% native β-CD HBA provided the highest enrichment factors of analytes compared to SUPRADESs comprised of other derivatives of β-CD (random methylated β-cyclodextrin, heptakis(2,3,6-tri-O-methyl)-β-cyclodextrin, and 2-hydroxypropyl β-cyclodextrin). In addition, native β-CD and its derivatives were dissolved in the neat DESs and their effect on the extraction of analytes examined. Dissolution of 20 wt% native β-CD in the choline chloride ([Ch + ][Cl - ]):2Urea DES resulted in a significant increase in the extraction efficiencies of target analytes compared to the neat [Ch + ][Cl - ]:2Urea DES. Under optimum conditions, the extraction method required a solvent microdroplet of 6.5 μL, 1000 rpm stir rate, 30% (w/v) salt concentration, and a temperature of 40 °C. The tetrabutylammonium chloride: 2 lactic acid DES resulted in the highest enrichment factors while the [Ch + ][Cl - ]:2Urea DES had the lowest for most of the analytes among the evaluated solvents. The method provided limits of detection (LODs) down to 35 μg L -1 . Finally, the developed method was applied for the analysis of spiked tap and lake water, where relative recoveries ranging from 83.7% -119.7% and relative standard deviations lower than 19.2% were achieved.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Evaluating Contributions of Pitch-Carbon Coating to Improved Stability of Si Anodes Through Voltage-Resolved Multi-Phase Characterization

Silicon nanoparticles have emerged as a promising alternative to graphite to improve the energy density of next-generation lithium-ion battery anodes. Nano-sized Si domains facilitate rapid ion transport and minimize particle-scale mechanical degradation, but also exhibit increased (electro)chemical reactivity with Li-ion electrolyte components due to their high surface area. We have previously demonstrated that surface modification of Si nanoparticles with pitch-carbon is an effective strategy to reduce these parasitic reactions. In the present work, we holistically evaluate the mechanistic contribution of pitch-carbon coating to the observed stability improvement over uncoated Si. We utilize coupled in situ and ex situ methods to probe changes to solid-surface, volatile headspace, and gas-phase chemistry occurring during initial cycling. Measurements taken at targeted potentials associated with electrolyte species reduction enables the decoupling of specific reaction pathways tied to interfacial stability. Further, we demonstrate the non-trivial role of gas reconsumption in dictating the nature of the passivating surface layer evolved on both uncoated and pitch-coated Si. This multi-phase analysis offers insights into the mechanism of effective surface passivation, which may be applied to inform future Si material development.

ENERGY STORAGE↗

Culture systems and methods of using same

Culture systems and methods of using same. The systems include a housing defining an inner space. The inner space includes a headspace and at least a portion of a reservoir. A surface for immobilizing cells is moveable between the headspace and the reservoir. The systems can be used for coculturing methanotrophs and phototrophs for processing biogas and wastewater, particularly from anaerobic digesters.

He, Qinghua↗

Methods of detecting predators in algal cultures

The present disclosure features methods of detecting crop damage in an algal culture. Such methods include detecting one or more carotenoids as a volatile organic compound in a sample obtained from a headspace of the algal culture.

Fisher, Carolyn Laura↗

Culture systems and methods of using same

Culture systems and methods of using same. The systems include a housing defining an inner space. The inner space includes a headspace and at least a portion of a reservoir. A surface for immobilizing cells is moveable between the headspace and the reservoir. The systems can be used for coculturing methanotrophs and phototrophs for processing biogas and wastewater, particularly from anaerobic digesters.

He, Qinghua↗

Initial Testing of an In Situ Load Retention Aging Vessel

A thermal aging vessel instrumented with load cells was fabricated. The primary function of the vessel is to continuously monitor the in situ load retention of up to three compressed polymer coupons undergoing thermally accelerated aging under nitrogen. A secondary function is to enable gas sampling of the vessel headspace during thermal aging. Heating of the vessel is achieved using a custom heater jacket. To improve upon our conventional aging study methods which require periodic interruption of aging to perform load testing in an Instron machine at room temperature, this technology aims to automate/facilitate data acquisition/analysis, improve data quality, and enable uninterrupted compression of the polymer which represents the service condition. As an example case to assess functionality of the in situ vessel, the load retention of a siloxane elastomer material additively manufactured by direct-ink-writing (DIW) was measured at three different isothermal aging temperatures for ~1 month. Initial compression of the coupons while near the aging temperature was achieved by temporarily opening the heated vessel to access the interior chamber and manually tightening four nuts to drive the heated compression plate down onto the heated coupons. Initial testing demonstrated achievement of the primary load retention monitoring function. Unfortunately, the vessel leaked which prevented gas sampling; an active purge was used to maintain a nitrogen atmosphere. Welded or otherwise sealed joints, which could be implemented in a future design, would likely eliminate leak paths. To apply time-temperature superposition (TTS), a technique used to provide long-term prediction of the load retention from short-term isothermal data, the load retention needed to be calculated relative to the load at an estimated “equilibrium” time, after most of the transient viscoelastic physical relaxation occurred. The peak load immediately after compression could not be used as the load retention basis for two reasons: (1) age-related changes must be isolated from non-age-related physical relaxation before applying TTS and (2) the manual mechanism used to compress the specimens at the aging temperature was neither smooth nor repeatable which affected the peak load value. To better understand the effect of the mode of initial compression on the measured load, and possibly better estimate “equilibrium” physical relaxation times, systematic stress relaxation experiments were performed using an Instron machine with a thermal chamber. At a given temperature, the DIW polymer was compressed to a fixed strain in either a stepped or continuous manner at two different rates, then held at that strain for 24 hrs. The results indicated that, at a given temperature, the different stress relaxation curves appeared to converge to the same curve at some “equilibrium” time when the non-age-related physical relaxation was mostly complete. Though this observation suggests that the discontinuous manual compression employed by the vessel is feasible, a compression mechanism that is rapid, smooth, and repeatable would enhance its use.

36 MATERIALS SCIENCE↗

Novel Foaming Solutions for High Level Waste (HLW) Processing - 20195

Foaming occurs during treatment of high level waste (HLW) at Savannah River Site's Defense Waste Processing Facility (DWPF) in the Chemical Process Cell (CPC) due to high gas generation from process steam and chemical offgas products [1]. The presence of amphiphilic particles in the waste slurry stabilizes the foam [2], [3]. Efficient processing of HLW requires foam control, as foam-overs lead to lower productivity and potential radioactive contamination of condensate streams. DWPF currently employs Siovation Antifoam 747, a surfactant produced by Momentive Performance Materials, as an antifoaming agent during waste treatment. Despite its ability to control foam generation, processing issues have arisen from its use [4]. During DWPF chemical processing, a chemical antifoam agent must be effective at temperatures up to 103 deg. C between pH 3-13. Antifoam 747 is effective at pH 7 but degrades as pH deviates [5]. Antifoam 747 is 90% by weight Momentive{sup TM} L77 and 10% by weight Momentive{sup TM} Y-17580. These ingredients are trisiloxane products, which are especially vulnerable to attack in acidic and caustic environments. Since Antifoam 747 readily degrades, periodic addition is required. Several processing concerns related to Antifoam 747 have affected DWPF operation. Its overuse warranted concern of potential flammable melter offgas under upset conditions due to the generation of carbon dioxide and hydrogen. As a result, a Potential Inadequacy in the Safety Analysis (PISA) was declared [6]. Antifoam contribution has been included in the melter offgas flammability strategy and the quantity of antifoam is monitored to ensure limits are not exceeded. Testing at Savannah River National Laboratory (SRNL) determined that propanal, tri-methylsilanol, and hexamethyldisiloxane are generated as Antifoam 747 degrades, leading to a second PISA [7]. The formation of these byproducts poses additional flammability risks. Furthermore, the methyl and ethyl groups of these compounds may be responsible for the formation of the methyl and ethyl mercury discovered in DWPF [8], [9]. The formation of organomercury has specifically been called out by DOE as a need for increased research. The effectiveness of non-chemical methods for foam control and the efficiency of alternative antifoam agents were evaluated as part of an effort to improve HLW treatment operations at DWPF and to reduce, or eliminate, the flammability hazards associated with Antifoam 747 currently in use. Foaming of high-level waste (HLW) slurries is an issue at the Defense Waste Processing Facility (DWPF) Chemical Process Cell (CPC) which is currently mitigated with a chemical antifoam agent. The effectiveness of non-chemical methods for foam control and the efficiency of alternative antifoams were examined to improve HLW treatment at DWPF and to eliminate the flammability hazards associated with Siovation Antifoam 747 currently in use. Non-chemical foam control methods were deemed unviable for chemical processing at DWPF, as the spray/mist technique requires too much water and space limitations make installation and implementation of headspace agitators unfeasible. The use of ultrasonic energy thickened and further stabilized the foam. Two suitable alternative defoaming agents, Momentive{sup TM} Y- 17112 and Evonik Surfynol{sup R} MD-20, were identified. Both defoamers control foam over a pH range of 4- 13 at boiling, with no flammable degradation products, and only minimal quantities (100-200 mg/kg) are required under glycolic acid conditions. In order to validate the effectiveness of these defoaming agents, SRNL recommends irradiation testing and laboratory scale SRAT/SME experiments with actual radioactive waste. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Mercury speciation using microcolumns with a direct mercury analyzer (DMA). Development of analytical method for the Savannah River Site liquid system

Mercury in the Savannah River Site (SRS) Liquid Waste System (LWS) exists in various forms, including: a) ionic inorganic mercury, organomercury (e.g., methyl Hg), and other less abundant species dissolved in LWS fluids, b) mercury solids such as oxides, hydroxides, amalgams, sulfides, and sorbed mercury, c) accumulations of dense liquid elemental mercury, and d) vapor phase elemental and organomercury mercury in tank headspace gas and in evaporators. Strategic and proactive management of the estimated 60,000 Kg mercury in the LWS requires deployment of efficient and effective paradigms for sampling and analysis of the total quantity of mercury in the various physical-chemical forms. Scoping tests of selective gas-phase sorbents for mercury speciation were performed to support LWS objectives. This research specifically focused on developing and testing streamlined methods to obtain high-quality analytical results for gaseous mercury species. The proposed methods are straightforward, using small columns (microcolumns) filled with materials that selectively sorb one or more target forms of mercury. Simple differentiation of mercury species and quantification is then achieved using an efficient thermal-desorption-based total mercury analyzer as the final step. Benefits associated with transitioning from multistep procedures such as EPA Methods 245.1, 1630 and 1631to streamlined microcolumn approaches include reduced analysis time, labor, and waste generation. Such transitioning would maximize the value of the current deployment of direct mercury analysis (EPA Method 7473) at SRS. This work has two target end uses: 1) simplifying the analysis steps and reducing costs for liquid samples (e.g., developing a total organic mercury (TOM) method), and 2) providing options for high-quality onsite analysis and rapid turnaround for gas samples in support of SRS LWS industrial hygiene (IH) objectives.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Deep eutectic solvents as green and sustainable diluents in headspace gas chromatography for the determination of trace level genotoxic impurities in pharmaceuticals

Genotoxic impurities (GTIs) are potential carcinogens that need to be controlled down to ppm or lower concentration levels in pharmaceuticals under strict regulations. The static headspace gas chromatography (HS-GC) coupled with electron capture detection (ECD) is an effective approach to monitor halogenated and nitroaromatic genotoxins. Deep eutectic solvents (DESs) possess tunable physico-chemical properties and low vapor pressure for HS-GC methods. In this study, zwitterionic and non-ionic DESs have been used for the first time to develop and validate a sensitive analytical method for the analysis of 24 genotoxins at sub-ppm concentrations. Compared to non-ionic diluents, zwitterionic DESs produced exceptional analytical performance and the betaine: 7 (1,4- butane diol) DES outperformed the betaine: 5 (1,4-butane diol) DES. Limits of detection (LOD) down to the 5-ppb concentration level were achieved in DESs. Wide linear ranges spanning over 5 orders of magnitude (0.005–100 µg g –1 ) were obtained for most analytes with exceptional sensitivities and high precision. The method accuracy and precision were validated using 3 commercially available drug substances and excellent recoveries were obtained. Finally, this study broadens the applicability of HS-GC in the determination of less volatile GTIs by establishing DESs as viable diluent substitutes for organic solvents in routine pharmaceutical analysis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Hydrogen Mitigation Process Installation at Nevada Solar One

The National Renewable Energy Laboratory (NREL) and Acciona Solar Power (ASP) have developed and are implementing a process that addresses the issue of hydrogen buildup in parabolic trough power plants. Our method selectively removes hydrogen from the expansion tanks of the power plant to control hydrogen levels in the circulating heat-transfer fluid (HTF). During previous work, we developed a sensor that measures hydrogen partial pressure in the expansion-tank headspace gas. We demonstrated that our sensor measures hydrogen levels over a wide range of partial pressure—from 1.33 mbar down to 0.003 mbar. More recently, we conceived and developed an integrated process module that performs both hydrogen sensing and separating functions. The sensor/separator measures hydrogen partial pressure in the headspace gas in the same way as our original sensor design. Additionally, the integrated module separates hydrogen from the headspace gas to reduce hydrogen to the level needed to maintain the performance of receivers in the collector field. We demonstrated the performance of a laboratory-scale version of this module. Testing showed that the module performed as expected: the accuracy of the sensing function was ±7%, and the hydrogen extraction rate for the separating mode was consistent with our modeling predictions. The primary benefit of this module is its simple design, both in terms of function and incorporation into the HTF subsystem of the power plant. Most recently, NREL and ASP planned, specified, and designed a mitigation process that is based on the integrated module. We are currently completing installation of this process at ASP's Nevada Solar One power plant in Boulder City, Nevada, USA. The mitigation process is being installed at ground level below the HTF expansion tanks, where it draws headspace gas from the tanks, removes hydrogen, and returns the treated gas back to the tanks. In this paper, we report progress on the installation and describe some of the many design details and challenges that we addressed during the past year. We will generate initial performance data from the Nevada Solar One mitigation process in early 2020.

41 EE - Solar Energy Technologies Office (EE-4S)↗

Hydrogen Mitigation Process Testing at Nevada Solar One

The National Renewable Energy Laboratory (NREL) and Acciona Solar Power (ASP) developed and installed a process that addresses the issue of hydrogen buildup in Acciona's Nevada Solar One power plant. Our method selectively removes hydrogen from the expansion tanks of the power plant to control hydrogen levels in the circulating heat-transfer fluid (HTF). During previous work, we developed a sensor that measures hydrogen partial pressure in the expansion-tank headspace gas. We demonstrated that our sensor measures hydrogen levels over a wide range of partial pressure from 10 mbar down to 0.003 mbar. More recently, we conceived and developed an integrated process module that performs both hydrogen sensing and separating functions. The sensor/separator measures hydrogen partial pressure in the headspace gas in the same way as our original sensor design. Additionally, the integrated module separates hydrogen from the headspace gas to reduce hydrogen to the level needed to maintain the performance of receivers in the collector field. Laboratory testing at NREL showed that the sensor function had an accuracy of +/-7%, and the hydrogen extraction rate for separator function was consistent with our modeling predictions. The primary benefit of this module is its simple design, both in terms of function and incorporation into the HTF subsystem of the power plant. Most recently, NREL and ASP completed installation and initial testing of a mitigation process at ASP's Nevada Solar One power plant in Boulder City, Nevada. In this paper, we report on the completed installation, initial testing, and plans to bring the process to full automation, so that it can be operated unattended on a daily schedule.

chemical elements↗

Identifying Challenges in Safeguards for Metallic Fuel Fabrication Facilities

As new advanced reactors gain popularity, there is an increasing interest in metallic fuel fabrication for fast reactors. While metallic fuels themselves are not a new idea, as many of the first reactors employed metallic fuels, new designs, compositions, and fabrication methods are appearing throughout the nuclear community. As the interest grows and facilities are constructed, both domestic and international safeguards will need to be heavily involved to support safeguards-by-design (SBD) measures from the start. This work compiles a review of historical and modern fuel types and fabrication methods, fabrication processes, safeguards gaps, and potential safeguards solutions. Metallic nuclear fuel types have been around for many decades and were included in some of the first reactors including the Experimental Breeder Reactor (EBR)-I and -II, the Fermi 1 reactor, the Integral Fast Reactor (IFR), and the Dounreay Fast Reactor (DFR). These reactors used various compositions including pure uranium (U) metal, U-zirconium (Zr) alloys, plutonium (Pu)-aluminum (Al) alloys, U-fissium (Fs) alloys, U-Pu-Zr alloys, and U-molybdenum (Mo) alloys [1, 2, 3, 4, 5]. These small alloying additions are included to improve the material properties of the pure U metal. The alpha-phase U (stable below 661C) suffers elongation in one direction causing grain boundary cracking and increasing creep rate due to irradiation growth, thermal cycling, and preferential crystal orientation. It is ideal to utilize the gamma-phase U (typically stable above 769C) by adding small amounts of alloying elements such as Zr or Mo to stabilize this phase down to room temperature [3]. Additionally, some research has been focused on U with transuranic (TRU) elements present, typically coming from the used fuel recycling process. Including these elements in fast reactor fuel can aid in the reduction of nuclear waste by burning minor long-lived actinides. However, the additions of TRU elements can cause concerns to arise when trying to fabrication or safeguard metallic fuels. A typical metallic fuel element is shown in Figure 1. Sodium is added into the cladding to create a thermal bond between the fuel slug and cladding wall. The fuel slug is then inserted and the end plug is welded on to the top of the fuel element. A gas plenum is left to create a headspace for gaseous fission products to escape rather than continue to build in the fuel itself [1, 5]. Other fuel element geometries exist as well, such as the Lightbridge twisted cruciform geometry shown in Figure 2 [6]. This design allows for better cooling performance and provides room for fuel rod swelling without impacting the fuel rod diameter. There are many different fabrication methods for metallic fuels, which is one of the many benefits of these fuel types. Many of these fabrication methods are relatively easy and cost-efficient. The most popular fabrication method is injection casting, sometimes called vacuum induction melting (VIM), shown in Figure 3 [4, 8, 9, 7, 10]. This method was largely used for EBR-II fuel fabrication. The injection casting system is contained inside of a vessel consisting of a Y2O3-coated graphite crucible surrounded by an induction coil with ZrO2-coated quartz molds suspended above the crucible. The fuel feedstock is placed inside of the graphite crucible and melted using the induction furnace. The induction furnace utilizes a dual frequency with the high frequency melting the feedstock and the low frequency causing stirring of the melted feedstock to form a homogeneous mixture. The mixture is heated to approximately 1600C in an argon environment. The vessel is evacuated and then the quartz molds are lowered into the graphite crucible containing the molten metal and the vessel is repressurized to inject the metal fuel upwards into the molds. The molds are removed and then shattered to release the fuel slugs. This fabrication method was used to fabricate 39,000 metallic fuel pins for EBR-II. While injection casting has been the most common metallic fuel fabrication method throughout the decades, many other methods have been explored including low-pressure gravity casting, microwave casting, continuous casting, centrifugal casting, coextrusion, and many others [11, 12, 8, 13, 14, 15]. Some of these methods aim to mitigate challenges that arise with americium (Am) volatilization during the casting process for TRU-containing fuel feedstocks, an issue with injection casting. Coextrusion is one of the methods explored at the Idaho National Laboratory (INL) and has been utilized for the initial fabrication tests of Lightbridge's unique fuels, as well as other metallic fuels with cladding coextruded. In this process, large billets are formed and machined and then inserted into a molten salt bath for approximately 30 minutes. The billets are then loaded into the extrusion press and extruded. This process can be seen in Figure 4 [15].

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Fe(III) reducing bacterial activities in Old Woman Creek wetland sediments, June 2023

To evaluate the Fe(III) reducing microbiological activities in Old Woman Creek Nature Preserve (OWC) wetland sediments, we incubated OWC sediments under anoxic and oxic conditions and with or without Fe(III) amendment [as hydrous ferric oxide (HFO)]. No Fe(III) reduction was observed in heat-deactivated incubations. In non-sterile anoxic incubations, measurement of 0.5 M HCl-extractable Fe(II) indicated that Fe(III) reduction occurred in both Fe(III)-amended and -unamended incubations, indicating that abundant Fe(III) is associated with the OWC sediments. Little Fe(II) accumulated in solution, indicating that the most biogenic Fe(II) adsorbs to the sediments. When air was added to the headspace of non-sterile incubations, Fe(III) reduction was halted and any biogenic Fe(II) that accumulated was oxidized. These experiments were used to guide preparation and analyses of incubations to determine if electrochemical measuements can be used to detect microbiological activities in contrasting terminal electron accepting regimes (i.e., aerobic and Fe(III) reducing conditions). Data package includes methods and data from experiments, including dissolved anion concentrations, dissolved Fe(II) concentrations, and 0.5 M HCl-extractable Fe(II) concentrations. All files are either .txt or .csv and can be opened by any plain text editor application.

EARTH SCIENCE↗

Light-Dependence of Formate (C1) and Acetate (C2) Transport and Oxidation in Poplar Trees

Although apparent light inhibition of leaf day respiration is a widespread reported phenomenon, the mechanisms involved, including utilization of alternate respiratory pathways and substrates and light inhibition of TCA cycle enzymes are under active investigation. Recently, acetate fermentation was highlighted as a key drought survival strategy mediated through protein acetylation and jasmonate signaling. Here, we evaluate the light-dependence of acetate transport and assimilation in Populus trichocarpa trees using the dynamic xylem solution injection (DXSI) method developed here for continuous studies of C1 and C2 organic acid transport and light-dependent metabolism. Over 7 days, 1.0 L of [13C]formate and [13C2]acetate solutions were delivered to the stem base of 2-year old potted poplar trees, while continuous diurnal observations were made in the canopy of CO2, H2O, and isoprene gas exchange together with δ13CO2. Stem base injection of 10 mM [13C2]acetate induced an overall pattern of canopy branch headspace 13CO2 enrichment (δ13CO2 +27‰) with a diurnal structure in δ13CO2 reaching a mid-day minimum followed by a maximum shortly after darkening where δ13CO2 values rapidly increased up to +12‰. In contrast, 50 mM injections of [13C]formate were required to reach similar δ13CO2 enrichment levels in the canopy with δ13CO2 following diurnal patterns of transpiration. Illuminated leaves of detached poplar branches pretreated with 10 mM [13C2]acetate showed lower δ13CO2 (+20‰) compared to leaves treated with 10 mM [13C]formate (+320‰), the opposite pattern observed at the whole plant scale. Following dark/light cycles at the leaf-scale, rapid, strong, and reversible enhancements in headspace δ13CO2 by up to +60‰ were observed in [13C2]acetate-treated leaves which showed enhanced dihydrojasmonic acid and TCA cycle intermediate concentrations. The results are consistent with acetate in the transpiration stream as an effective activator of the jasmonate signaling pathway and respiratory substrate. The shorter lifetime of formate relative to acetate in the transpiration stream suggests rapid formate oxidation to CO2 during transport to the canopy. In contrast, acetate is efficiently transported to the canopy where an increased allocation towards mitochondrial dark respiration occurs at night. The results highlight the potential for an effective integration of acetate into glyoxylate and TCA cycles and the light-inhibition of citrate synthase as a potential regulatory mechanism controlling the diurnal allocation of acetate between anabolic and catabolic processes.

59 BASIC BIOLOGICAL SCIENCES↗

Differential Organic Carbon Mineralization Responses to Soil Moisture in Three Different Soil Orders Under Mixed Forested System: Supporting Data

This data contains data from 90-day long incubation study which aimed to look at the soil moisture-texture relationship on soil organic carbon (SOC) cycling. Soils were collected from three distinct soil textures from mixed forests in 2017: sandy (Georgia, 2017-05-01), loamy (Missouri, 2017-06-14) and clayey (Texas, December 2017) were incubated at different soil moisture levels (air-dried, 25% water holding capacity (WHC), 50% WHC, 100% WHC and 175% WHC) at room temperature for a period of 90 days. Files contain microbial respiration, active and slow SOC pools, and their respective mineralization rates, extractable organic carbon (C), and C-acquiring extracellular enzymes. Findings from these data were used in Singh et al. (2021). This study aimed to examine the interactive effect of soil moisture and texture on SOC mineralization. Soil samples of three distinct textures (sandy, loamy, and clayey) were collected from mixed forests of Georgia, Missouri, and Texas, respectively. Soil cores of 5 cm diameter were collected from numerous random locations at each site from 0-15 cm depth after scraping the litter layer and mixed thoroughly to obtain a composite sample per site. Three additional soil cores were collected to determine the WHC using pressure plate extractors. Soil samples were composited, and triplicate soil samples were incubated in mason jars for a period of 90 days at room temperature under different moisture regimes: air dried, 25% WHC, 50% WHC, at WHC and 100% saturation. Soil respiration was measured weekly, and destructive sampling was conducted at 1, 15, 60, and 90 days to determine extractable organic C, C acquiring enzyme activity, and active and slow SOC pools with their respective mineralization rates. The C acquiring enzyme activity was the total activity of α-glucosidase, β-glucosidase, cellobiohydrolase, and β-xylosidase enzymes. Gas samples for microbial respiration measurements were collected from headspace of incubation jars through the sampling ports on the lids and then analyzed using a Shimadzu Gas Chromatograph (GC-2014). Prior to sampling, the vials were evacuated. Blank correction was also done by collecting gas samples from empty incubation jars. Double pool exponential decay model was used in SigmaPlot to determine the active and slow SOC pools and their mineralization rates (Farrar et al., 2012; Jagadamma et al., 2014). The C-acquiring extracellular enzymes were measured using the microplate method by German et al., (2011). Microbial community structure was determined using the phospholipid fatty acid (PLFA) and neutral lipid fatty acid (NLFA) analyses (Buyer and Sasser, 2012). This dataset has seven data files provided in comma-separate (*.csv) format. Additional metadata are provided: seven data dictionaries and a file-level metadata file in comma separate (*.csv) format and a user guide in PDF (*.pdf) format.

Carbon acquiring enzyme activity↗