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NASA NTRS2016

A Fly-Through Mission Strategy Targeting Peptide as a Signature of Chemical Evolution and Possible Life in Enceladus Plumes

In situ detection of organic molecules in the extraterrestrial environment provides a key step towards better understanding the variety and the distribution of building blocks of life and it may ultimately lead to finding extraterrestrial life within the Solar System. Here we present combined results of two separate experiments that enable us to realize such in situ life signature detection from the deep habitats of the "Ocean World": a hydrothermal reactor experiment simulating complex organic synthesis and a simulated fly-through capture experiment of organic-bearing microparticles using silica aerogels, followed by subsequent analysis. Both experiments employ peptide as a plausible organics existing in Encleadus plume particles produced in its subsurface ocean. Recent laboratory hydrothermal experiments and a theoretical model on silica saturation indicated an on going hydrothermal reactions in subsurface Enceladus ocean. Given the porous chondritic origin of the core, it is likely that organic compounds originated by radiation chemistry such as amino acid precursors could have been provided, leached, and altered through widespread water-rock interactions. By using the same laboratory experimental setup from the latest water-rock interaction study, we performed amino acid polymerization experiments for 144 days and monitored the organic complexity changing over time. So far over 3,000 peaks up to the size of greater than 600 MW were observed through the analysis of capillary electrophoresis time-of-flight mass spectrometry (CE-TOF-MS) with an indication of amino acid derivatives and short peptides. Generally abiotic polymerization of enantiomeric amino acids results in forming stereoisomeric peptides with identical molecular weight and formula as opposed to homochiral biopolymers. Assuming Enceladus plume particles may contain a mixture of stereoisomeric peptides, we were able to distinguish 16 of the 17 stereoisomeric tripeptides as a test sample using capillary electrophoresis (CE) under optimized conditions. We further conducted Enceladus plume fly-through capture experiment by accelerating peptides soaked in rock particles up to a speed of 5.7 km/s and capturing with originally developed hydrophobic silica aerogels. Direct peptide extraction with acetonitrile-water followed by CE analysis led to detection of only but two stereoisomeric acidic peptide peaks, presenting the first run-through hypervelocuty impact sample analysis targeting peptides as key molecule to to understand the ongoing astrobiology on Enceladus.

organic molecules↗

DOE OSTI2023

Challenges and Advances in Aqueous Processing of Corn Stover Pellets into High Concentration Slurries

Significant progress has occurred in developing combined enzyme hydrolysis and fermentation technologies for transforming lignocellulosic feedstocks into ethanol and other bioproducts. Various routes described in the literature show that low carbon footprint processes efficiently convert the cellulose and hemicellulose fractions of pretreated corn stover, wood chips, and sugarcane bagasse to sugars and to ethanol.Combinations of different pretreatments at high or low pH or in liquid hot water, followed by enzyme hydrolysis and fermentation or direct conversion of cellulose to ethanol (i.e., by consolidated bioprocessing)have been demonstrated. These successes have brought the need to preparing the feedstock – before it enters the biorefinery – into focus. This paper summarizes recent developments in liquefying corn stover,before pretreatment, so that slurries with yield stresses below 200 Pa are obtained and a “pumpable” corn stover slurry results at initial solids loadings of up to 300 g/L. The manner in which corn stover pellets are combined with water and enzyme in an agitated bioreactor is described, and properties that define slurry behavior are presented. Implications on biorefinery operations are explained in terms of particle properties and the preprocessing of corn stover as well as the team approach used to obtain these results.

Wassgren, Carl↗

DOE OSTI2023

Engineering osmolysis susceptibility in Cupriavidus necator and Escherichia coli for recovery of intracellular products

Intracellular biomacromolecules, such as industrial enzymes and biopolymers, represent an important class of bio-derived products obtained from bacterial hosts. A common key step in the downstream separation of these biomolecules is lysis of the bacterial cell wall to effect release of cytoplasmic contents. Cell lysis is typically achieved either through mechanical disruption or reagent-based methods, which introduce issues of energy demand, material needs, high costs, and scaling problems. Osmolysis, a cell lysis method that relies on hypoosmotic downshock upon resuspension of cells in distilled water, has been applied for bioseparation of intracellular products from extreme halophiles and mammalian cells. However, most industrial bacterial strains are non-halotolerant and relatively resistant to hypoosmotic cell lysis. To overcome this limitation, we developed two strategies to increase the susceptibility of non-halotolerant hosts to osmolysis using Cupriavidus necator, a strain often used in electromicrobial production, as a prototypical strain. In one strategy, C. necator was evolved to increase its halotolerance from 1.5% to 3.25% (w/v) NaCl through adaptive laboratory evolution, and genes potentially responsible for this phenotypic change were identified by whole genome sequencing. The evolved halotolerant strain experienced an osmolytic efficiency of 47% in distilled water following growth in 3% (w/v) NaCl. In a second strategy, the cells were made susceptible to osmolysis by knocking out the large-conductance mechanosensitive channel (mscL) gene in C. necator. When these strategies were combined by knocking out the mscL gene from the evolved halotolerant strain, greater than 90% osmolytic efficiency was observed upon osmotic downshock. A modified version of this strategy was applied to E. coli BL21 by deleting the mscL and mscS (small-conductance mechanosensitive channel) genes. When grown in medium with 4% NaCl and subsequently resuspended in distilled water, this engineered strain experienced 75% cell lysis, although decreases in cell growth rate due to higher salt concentrations were observed. Our strategy is shown to be a simple and effective way to lyse cells for the purification of intracellular biomacromolecules and may be applicable in many bacteria used for bioproduction.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2023

Carbon, Nitrogen, and Sulfur Analysis of the Cetama Viognier Standard Reference Material

The Viognier sample was analyzed for C, N, and S concentrations and stable isotope compositions using an Elementar Vario Isotope Cube Elemental Analyzer (EA) that is coupled to an IsoPrime PrecisION IRMS. Powder samples were placed in tin capsules and then loaded onto a rotary autosampler. The autosampler dropped samples into the EA, and samples were combusted at 1175 °C over tungsten oxide in a continuous stream of helium carrier gas. A pulse of oxygen is added to the gas stream resulting in flash combustion of the tin capsule containing the sample, which raises the reaction temperature to approximately 1800 °C for a few seconds. The combustion reaction produces SO 2 , N 2 and CO 2 from any sulfur, nitrogen and carbon present in the sample. The resulting gases were then passed through a reduced copper reactor that was heated to 850 °C, to reduce NO x to N 2 , reduce SO 3 to SO 2 , and trap any volatile halogen compounds on silver wool. Following water removal using an adsorption tube, the N 2 , CO 2 , and SO 2 analyte gases were separated and purified using purge-trap columns. The purified gases were then carried through a thermal conductivity detector. The detector signal was passed to software that calculated elemental abundances based on integrated peak areas. The sample gases were then passed to the IRMS and stable isotope ratios were measured. Raw sample peak areas were corrected by subtracting the average peak area from blanks consisting of empty tin capsules run using the same EA analysis method. Blanks were also run following each replicate to verify that all the material was combusted. The Viognier sample was analyzed in triplicate on two days (target sample masses: 30, 60 and 90 mg). The following standards were analyzed to calibrate EA-IRMS measurements: IAEA-C6, USGS-40, USGS-41, IAEA-S1, and IAEA-S2.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2021

Catalytic Activity and Water Stability of the MgO(111) Surface for 2-Pentanone Condensation

Nanomaterials derived from earth-abundant metal oxides have gained tremendous interest as catalysts; although, water stability remains a challenge. This study examines MgO(111) surfaces for 2-pentanone condensation and their evolution during D2O hydration. Catalyst screening confirmed the high activity of fresh MgO(111) for 2-pentanone condensation relative to conventionally prepared MgO(100). Computational modeling suggests that the (111) surface is readily hydroxylated, and that surface hydroxyls help stabilize the surface and reduce the barrier for 2-pentanone condensation. Vapor-phase D2O hydration after 3 min increased MgO(111) hydroxyls and retained surface area and activity; however, after 1 h, deuteroxide formation reduced the surface area and activity by >30 %. After 24 h, deuteroxide growth slowed down, and surface area and activity remained stable. This suggests MgO(111)-derived hydroxide may be the dominant surface responsible for 2-pentanone condensation following water exposure. Thermal regeneration of the 24-h sample restored 86 % of the surface area and 94 % of the activity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Mark-18A Cold Runs

The Savannah River National Laboratory (SRNL) is tasked by the National Nuclear Security Administration (NNSA) to recover highly valued isotopes from irradiated Mark-18A (Mk-18A) targets. The Savannah River Site (SRS) has sixty-five Mk-18A targets available for the recovery of the high valued materials. The sixty-five Mk-18A targets are currently stored in the L-Area Basin and will be removed one at a time and individually transported to SRNL. Upon receipt at SRNL, the Mk-18A target material will be removed from the confinement, dissolved, chemically separated, and calcined to a stable oxide. The flowsheet is designed to recover the plutonium as well as the trivalent actinides. The remaining unrecovered material will be discarded to the high activity drain (HAD) system in SRNL. A specially designed cask was procured for transport of the targets from L-Area to SRNL. Once received at SRNL, the targets will be loaded into the back of Cell 7 and resized as they enter the cell. The resized targets (1/4 lengths) will then be processed one at a time through the following processes: caustic dissolution and filtration; acidic dissolution and filtration, Reillex anion exchange, diglycolamide (DGA) cation exchange; and DGA calcination. This processing will result in two product streams. The first is an aqueous plutonium solution which will be removed from the shielded cells and taken to a glovebox for further purification and conversion to an oxide. The second is a calcined oxide containing the Am and Cm as well as other lanthanide fission products which will be removed from the shielded cells using a bagless transfer system. Both materials will be packaged for shipment to Oak Ridge National Laboratory (ORNL). All equipment to carry out this process was designed, procured or fabricated, and installed in a mock-up facility (716-4A) at SRS to allow for simulation testing in a non-radioactive area. This equipment was then dismantled and transferred from 716-4A to 773-A and installed in the SRNL Shielded Cells. After installation in the shielded cells facility testing was performed using water followed by surrogates and cold chemicals. Issues were identified during these evaluations, including equipment issues as well as technical challenges. Many of the issues were rectified during performance of the cold runs, and the remaining have a resolution identified. Table ES-1 provides a summary of all issues identified during the cold run operations, as well as the status and identified resolutions to outstanding issues.

07 ISOTOPE AND RADIATION SOURCES↗

DOE OSTI2020

Variability in structural carbohydrates, lipid composition, and cellulosic sugar production from industrial hemp varieties

The aim of this study was to determine carbohydrate recovery from hemp for ethanol production and quantify biodiesel from TAG (Triacylglycerol) present in hemp. The structural composition of five different hemp varieties (Seward County-SC, York County-YC, Loup County-LC, 19 m96136-19 m, and CBD Hemp-CBD) were analyzed. Concentration of glucan and xylan ranged between 32.63 to 44.52% and 10.62 to 15.48% respectively. The biomass was then pretreated with Liquid hot water followed by disk milling and then hydrolyzed enzymatically to yield monomeric sugars. High glucose (63-85%) and xylose (73-88%) recovery was achieved. Lipids were extracted from hemp using hexane and isopropanol and then transesterified to produce biodiesel. Approximately, 50% of total fatty acids in SC, LC, and CBD hemp were linoleic acid. Palmitic acid was present between 32 to 50% in varieties YC and 19 m. Highest TAG concentration at 25% of total lipids was observed in CBD hemp. In conclusion, the analysis on lipid composition and high sugar recovery demonstrates hemp as a potential bioenergy crop for ethanol and biodiesel coproduction.

09 BIOMASS FUELS↗

DOE OSTI2022

Integration of Highly Luminescent Lead Halide Perovskite Nanocrystals on Transparent Lead Halide Nanowire Waveguides through Morphological Transformation and Spontaneous Growth in Water

The integration of highly luminescent CsPbBr 3 quantum dots on nanowire waveguides has enormous potential applications in nanophotonics, optical sensing and quantum communications. On the other hand, CsPb 2 Br 5 nanowires have also attracted a lot of attention due to their unique water stability and controversial luminescent property. Here we first report the growth of CsPbBr 3 nanocrystals on CsPb 2 Br 5 nanowires by simply immersing CsPbBr 3 powder into pure water, CsPbBr 3-γ X γ (X = Cl, I) nanocrystals on CsPb 2 Br 5-γ X γ nanowires are then synthesized for tunable light sources. Systematic structure and morphology studies, including in-situ monitoring, revealed that CsPbBr 3 powder was first converted to CsPb 2 Br 5 microplatelets in water, followed by a morphological transformation from CsPb 2 Br 5 microplatelets to nanowires, which is a kinetic dissolution-recrystallization process controlled by electrolytic dissociation and supersaturation of CsPb 2 Br 5 . CsPbB r3 nanocrystals are spontaneously formed on CsPb 2 Br 5 nanowires when nanowires are collected from the aqueous solution. Raman spectroscopy, combined photoluminescence and SEM imaging confirm that the bright emission originates from CsPbBr 3-γ X γ nanocrystals while CsPb 2 Br 5-γ X γ nanowires are transparent waveguides. In conclusion, the intimate integration of nanoscale light sources with a nanowire waveguide is demonstrated through the observation of the wave guiding of light from nanocrystals and Fabry-Perot interference modes of the nanowire cavity.

42 ENGINEERING↗

DOE OSTI2023

Batch Scale Production of 3D Printed Extraction Sorbents Using a Low-Cost Modification to a Desktop Printer

This study reports a simple modification to a commercial resin 3D printer that significantly reduces the amount of prepolymer material needed for the production of extraction sorbents. Here, the modified printing platform is demonstrated in the printing of two imidazolium-based ionic liquid (IL) monomers. Two geometries resembling a blade-type polymeric ionic liquid (PIL) sorbent used in thin-film microextraction and a fiber-type sorbent used in solid-phase microextraction (SPME) were printed. The SPME PIL sorbents were used to extract 10 organic contaminants, including plasticizers, antimicrobial agents, UV filters, and pesticides, from water followed by high-performance liquid chromatographic (HPLC) analysis. To compare the extraction performance of the SPME sorbents, seven fibers printed with the same prepolymer composition from the same printing batch as well as different batches were evaluated. The results revealed highly reproducible extraction efficiencies for all tested sorbents with no statistical difference in their extraction performance. Method validation showed acceptable linearity ($R$ 2 > 0.92) for all analytes with limits of detection and limits of quantification ranging from 0.13 to 45 μg L –1 and 0.43 to 150 μg L –1 , respectively.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Extreme Ultraviolet and Beyond Extreme Ultraviolet Lithography Using Amorphous Zeolitic Imidazolate Resists Deposited by Atomic/Molecular Layer Deposition

Amorphous zinc-imidazolate (aZnMIm) resists show potential to meet the demands for next-generation high-numerical aperture (high-NA) metal-containing extreme ultraviolet (EUV) resist materials, given their ease of deposition by atomic/molecular layer deposition (ALD/MLD) at thicknesses of 20 nm and below. Here, this study demonstrates that aZnMIm thin films, previously identified as high-resolution electron beam resists, can also function as negative-tone EUV photoresists. Water development achieves high sensitivity (5 mJ/cm 2 ) but leaves significant residue, while acetic acid development results in poor contrast. A hybrid approach─water followed by acetic acid─enables residue-free development with a sensitivity of 181 mJ/cm 2 . Dry development using 1,1,1,5,5,5-hexafluoroacetylacetone (hfacH) is also possible but shows lower sensitivity (375 mJ/cm 2 ) compared to wet development methods. EUV photoelectron spectroscopy (PES), reflectometry/EUV absorption, total electron yield (TEY), residual gas analysis (RGA), and time-of-flight secondary ion mass spectrometry (TOF-SIMS) were used to investigate the effects of EUV irradiation on aZnMIm resists. Reflectometry experiments reveal an aZnMIm EUV absorption coefficient of 6.2 μm –1 , while PES and TEY analyses show that, compared to poly(4-hydroxystyrene) (PHS), a polymer-based reference resist, aZnMIm emits more primary and secondary electrons but generates fewer slow electrons relative to its primary electron emission; its total electron yield is similar to that of poly(methyl methacrylate) (PMMA) resists. When exposed to EUV, aZnMIm predominantly outgasses H 2 , as determined by RGA. TOF-SIMS measurements demonstrate that high-dose EUV exposure only partially fragments the 2-methylimidazole (2MIm) organic linkers, unlike high-dose electron beam exposure, which is known to completely degrade them. Additionally, aZnMIm resists show promise for potential beyond EUV lithography (BEUVL) due to the presence of Zn, which provides higher sensitivity at a wavelength of 6.7 nm compared to other metal ions, such as Sn, that are currently used in the best-performing EUV metal–organic resists. TEY measurements demonstrate that aZnMIm emits nearly twice as many electrons as PHS at 6.7 nm. The BEUV TEY of aZnMIm also surpasses that of PMMA, poly(pentafluorostyrene), and poly(4-iodostyrene), with the latter two being known for their high EUV TEYs. This work provides insight into zeolitic imidazolate framework (ZIF)-based EUV and BEUV resists and highlights their potential for both wet and dry development.

lithography↗

DOE OSTI2021

Reactive Species and Reaction Pathways for the Oxidative Cleavage of 4-Octene and Oleic Acid with H 2 O 2 over Tungsten Oxide Catalysts

The oxidative cleavage of carbon-carbon double bonds (C=C) in alkenes and fatty acids produces aldehydes and acids valued as chemical intermediates. Solid tungsten oxide catalysts are low cost, non-toxic, and selective for the oxidative cleavage of C=C bonds with hydrogen peroxide (H 2 O 2 ) and are, therefore, a promising option for continuous processes. Despite the relevance of these materials, the elementary steps involved and their sensitivity to the form of W sites present on surfaces have not been described. In this work, we combine in situ spectroscopy and rate measurements to identify significant steps in the reaction, the reactive species present on catalysts, and examine differences between the kinetics of this reaction on isolated W atoms grafted to alumina and on those exposed on crystalline WO 3 nanoparticles. Raman spectroscopy shows that W-peroxo complexes (W-(η 2 -O 2 ) formed from H 2 O 2 ) react in a kinetically relevant step to produce epoxides, which undergo hydrolysis at protic surface sites. Subsequently, the CH 3 CN solvent deprotonates diols to form alpha hydroxy ketones that react to form aldehydes and water following nucleophilic attack of H 2 O 2 . Turnover rates for oxidative cleavage, determined by in situ site titrations, on WO x -Al 2 O 3 are 75% greater than those on WO 3 at standard conditions. These differences reflect activation enthalpies (ΔH ‡ ) for oxidative cleavage of 4-octene that are much lower for the isolated WO x sites (36±3 and 60±6 kJ∙mol -1 for WO x -Al 2 O 3 and WO 3 , respectively) and correlate strongly with the difference between enthalpies of adsorption for epoxyoctane (ΔH ads,epox ), which resembles the transition state for epoxidation. The WO x -Al 2 O 3 catalysts mediate oxidative cleavage of oleic acid with H 2 O 2 following a mechanism comparable to that for 4-octene. The WO 3 materials, however, form only the epoxide and do not cleave the C-C bond or produce aldehydes and acids. These differences reflect the distinct site requirements for these reaction pathways and indicate that acid sites required for diol formation are strongly inhibited by oleic acids and epoxides on WO 3 whereas the Al 2 O 3 support provides sites competent for this reaction and increase the yield of the oxidative cleavage products.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Backbone-Photodegradable Polymers by Incorporating Acylsilane Monomers via Ring-Opening Metathesis Polymerization

Materials capable of degradation upon exposure to light hold promise in a diverse range of applications including biomedical devices and smart coatings. Despite the rapid access to macromolecules with diverse compositions and architectures enabled by ring-opening metathesis polymerization (ROMP), a general strategy to introduce facile photodegradability into these polymers is lacking. Here, we report copolymers synthesized via ROMP that can be degraded by cleaving the backbone in both solution and solid states under irradiation with a 52 W, 390 nm Kessil LED to generate heterotelechelic low-molecular-weight fragments. To the best of our knowledge, this work represents the first instance of the incorporation of acylsilanes into a polymer backbone. Mechanistic investigation of the degradation process supports the intermediacy of an α-siloxy carbene, formed via a 1,2-photo Brook rearrangement, which undergoes insertion into water followed by cleavage of the resulting hemiacetal.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Data for Variability in Structural Carbohydrates, Lipid Composition, and Cellulosic Sugar Production from Industrial Hemp Varieties

The aim of this study was to determine carbohydrate recovery from hemp for ethanol production and quantify biodiesel from TAG (triacylglycerol) present in hemp. The structural composition of five different hemp varieties (Seward County-SC, York County-YC, Loup County-LC, 19 m96136-19 m, and CBD Hemp-CBD) were analyzed. Concentration of glucan and xylan ranged between 32.63 to 44.52% and 10.62 to 15.48% respectively. The biomass was then pretreated with Liquid hot water followed by disk milling and then hydrolyzed enzymatically to yield monomeric sugars. High glucose (63-85%) and xylose (73-88%) recovery was achieved. Lipids were extracted from hemp using hexane and isopropanol and then transesterified to produce biodiesel. Approximately, 50% of total fatty acids in SC, LC, and CBD hemp were linoleic acid. Palmitic acid was present between 32 to 50% in varieties YC and 19 m. Highest TAG concentration at 25% of total lipids was observed in CBD hemp. The analysis on lipid composition and high sugar recovery demonstrates hemp as a potential bioenergy crop for ethanol and biodiesel coproduction.

Biomass Analytics↗

DOE OSTI2021

Data from Reactive Species and Reaction Pathways for the Oxidative Cleavage of 4-Octene and Oleic Acid with H2O2 over Tungsten Oxide Catalysts

Oxidative cleavage of carbon–carbon double bonds (C═C) in alkenes and fatty acids produces aldehydes and acids valued as chemical intermediates. Solid tungsten oxide catalysts are low cost, nontoxic, and selective for the oxidative cleavage of C═C bonds with hydrogen peroxide (H2O2) and are, therefore, a promising option for continuous processes. Despite the relevance of these materials, the elementary steps involved and their sensitivity to the form of W sites present on surfaces have not been described. Here, we combine in situ spectroscopy and rate measurements to identify significant steps in the reaction and the reactive species present on the catalysts and examine differences between the kinetics of this reaction on isolated W atoms grafted to alumina and on those exposed on crystalline WO3 nanoparticles. Raman spectroscopy shows that W–peroxo complexes (W–(η2-O2)) formed from H2O2 react with alkenes in a kinetically relevant step to produce epoxides, which undergo hydrolysis at protic surface sites. Subsequently, the CH3CN solvent deprotonates diols to form alpha-hydroxy ketones that react to form aldehydes and water following nucleophilic attack of H2O2. Turnover rates for oxidative cleavage, determined by in situ site titrations, on WOx–Al2O3 are 75% greater than those on WO3 at standard conditions. These differences reflect the activation enthalpies (ΔH‡) for the oxidative cleavage of 4-octene that are much lower than those for the isolated WOx sites (36 ± 3 and 60 ± 6 kJ·mol–1 for WOx–Al2O3 and WO3, respectively) and correlate strongly with the difference between the enthalpies of adsorption for epoxyoctane (ΔHads,epox), which resembles the transition state for epoxidation. The WOx–Al2O3 catalysts mediate oxidative cleavage of oleic acid with H2O2 following a mechanism comparable to that for the oxidative cleavage of 4-octene. The WO3 materials, however, form only the epoxide and do not cleave the C–C bond or produce aldehydes and acids. These differences reflect the distinct site requirements for these reaction pathways and indicate that acid sites required for diol formation are strongly inhibited by oleic acids and epoxides on WO3 whereas the Al2O3 support provides sites competent for this reaction and increase the yield of the oxidative cleavage products.

Catalysis↗

DOE OSTI2021

Geochemical Variation of Produced Waters and Overlying Groundwaters at an Active CO 2 Enhanced Oil Recovery Field in the Permian Basin Central Platform

This report discusses the results of baseline geochemical data from a carbon dioxide (CO 2 ) enhanced oil recovery (EOR) field in the Permian Basin’s Central Basin Platform. This report focuses on understanding the variability in geochemistry during normal oil field practices, including the transition from water flooding to a water-alternating-gas (WAG) technique. The primary objectives of this study were to focus on 1) determining the best general geochemical parameters to identify produced water intrusion into overlying groundwaters, 2) observing if there was any intrusion during the sampling period, and 3) identifying changes in produced water following CO 2 injection.

02 PETROLEUM↗

DOE OSTI2023

X-ray Pump-Probe Measurements using a Laser-Plasma Accelerator (Final Report)

This project funded one graduate student, Mario Balcazar, to perform experiments on high power laser facilities to study the application of X-rays generated by laser wakefield accelerated electrons for advanced radiography, in particular X-ray phase contrast imaging of hydrodynamic shocks/instabilities. The work made use of the DOE’s LaserNetUS facilities. We performed dynamic phase-contrast X-ray imaging of the shock generated by a 200 ps duration laser pulse (E = 1 J, I = 10 15 Wcm –2 ) with a 30 µm diameter liquid target, with unprecedented spatio-temporal resolution. This includes multi-shock generation within the liquid jet and plasma instability formation. Innovative electron-beam radiography was used to probe the laser-plasma interplay finding evidence of bilateral heating of the water followed by strong electric field generation. These measurements help explain some of the discrepancies between simulation and experiment and pave the way to better plasma diagnostic systems in HED and ICF physics experiments. This work was performed in collaboration with researchers from Michigan, LLNL, LBL and Sandia National Laboratories, Queen’s University Belfast and Imperial College.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2024

Cellulose molecular weight of corn stover with cotreatment

Here we present a dataset of cellulose molecular weights from corn stover after a cotreatment process. The corn stover sample was subjected to a combination of mechanical disruption (ball milling) and consolidated bioprocessing (CBP) process using the bacterium C. thermocellum at 60 grams/L solids loadings. Cellulose was isolated from control, no cotreatment control, and cotreatment corn stover. Cellulose was then derivatized using anhydrous pyridine and phenyl isocyanate over 48 h at 70 ºC. The reaction was quenched by anhydrous methanol. Methanol and water mixture (7:3, v/v) was added dropwise to promote precipitation of the cellulose derivative. The solids were collected by filtration and thoroughly washed with the methanol and water mixture followed by water. The cellulose derivative was dried overnight under vacuum at 40°C. The obtained cellulose tricarbanilates was then dissolved in tetrahydrofuran (THF) at 1.0 mg/mL and the solution was filtered through a 0.45 µm PTFE filter and placed in an auto-sampler vial. The molecular weight of cellulose was measured by Agilent GPC SECurity 1200 system equipped with four Waters Styragel columns (i.e., HR0.5, HR2, HR4, and HR6) and a UV detector (270 nm). THF was used as the mobile phase. Data collection and processing was performed by Polymer Standards Service WinGPC Unity software (Build 6807). The molecular weight was calculated relative to the polystyrene calibration curve. The data on molecular weights provided information about the effects of cotreatment on corn stover cellulose molecular changes.

Cellulose, molecular weights, corn stover, cotreat↗

NASA NTRS1972

Enzyme activity in terrestrial soil in relation to exploration of the Martian surface

Urease activity in soil is persistent for long periods under low water, low temperature, and sterile regimes, and it was suggested that some form of enzyme-protective mechanism exists in soil. Dublin soil was extracted by sonication in water followed by adding a mixture of salts. Urease activity is associated with the organo-mineral complex thus obtained and is resistant to the activities of proteolytic enzymes. Clay free soil organic matter prepared subsequently by filtration also exhibits urease activity which is resistant to proteolysis. Models consisting of enzymes with bentonite and lignin were found to mimic this resistance to proteolysis. A model system is presented which suggests both the origin and location of soil ureases and a reason for their persistence in nature.

Ardakani, M. S.↗