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DOE OSTI2023

Lignetics CRADA closeout report

Lignetics is one of the leading domestic producers of wood pellet fuels used for domestic heating. The company also produces pellets for other applications including animal bedding. The primary feedstock used for the production of Lignetics products is woody biomass. To improve the economics of pellet production, Lignetics is evaluating advanced preprocessing technologies developed by researchers at INL. In the proposed project, INL and Lignetics will work collaboratively to assess the feasibility of integrating INL’s advanced preprocessing technologies (fractional milling, high moisture pelleting and low temperature drying) in Lignetics production facilities. The successful completion of the project relies on the integration of the fractional milling and high moisture pelleting (HMP) process and low temperature drying to improve the economics of woody biomass pellet production for use in biofuel and bioproduct applications. In the HMP process, the biomass loses some moisture during compression and extrusion through the pellet die due frictional heat developed. Also, as pellets have a definite size and shape, they can be further dried in low temperature grain or belt dryers. Belt dryers are better suited to take advantage of low-grade and waste heat because they operate at lower temperatures than rotary dryers (Tumuluru et al.) Rotary dryers, for example, typically require inlet temperatures of 260°C, but more optimally operate around 400°C. In contrast, the inlet temperature of a belt dryer, such as a commercially available vacuum dryer, can be as low as 10°C above the ambient temperature, although more typically they operate at higher temperatures, between 90°C and 200°C. Because of their lower temperature operation, fire hazards and emissions to the air are lower for belt dryers in addition to reducing drying and overall pelleting costs, INL’s technology also has potential to reduce emissions at Lignetics facilities.

09 BIOMASS FUELS↗

DOE OSTI2022

Impact of anatomical fractionation of corn stover on hammer mill throughput and energy consumption

The goal of this Case Study was to quantify the impacts of variable moisture and ash on hammer mill throughput and energy consumption and on loss of very wet stover that causes failures in the first stage grinder and that are not able to be fed to conversion, as compared to a status quo Base Case system. Also considered was convertible carbohydrate content (minimum total carbohydrate specification) and maximum ash content and the delivered feedstock cost impacts of not being able to feed stover not meeting the total carbohydrate specification to the conversion reactor. Laboratory data on the impacts of moisture content and tissue fraction on throughput and energy consumption in a stage 2 hammer mill were received from FCIC Subtask 5.1. Additional air classifier throughput, energy consumption and separation efficiency data were obtained from FCIC Subtask 5.1 for the new air classifier, which has three exit streams (lights, middle and heavies). These data were utilized to develop the necessary response surface equations to perform throughput analysis using discrete event simulation. Because the ash contents and particle sizes had not been analyzed in the laboratory at the time of the model runs, we assumed that the ash distributed proportionally with total mass into the lights and heavies in an air classifier having two exit streams (lights and heavies) and that the lights fraction from the air classifier was not removed. Key takeaways from this Case Study are that due to lower energy consumption, it is more cost effective to hammer mill fractionated corn stover tissues than whole stover. Reduction of grinding energy was significant and may possibly be connected to particle-particle interactions in the grinder that lead to increased residence time of leaves and husks, resulting in decreased throughput and higher generation of fines when milling whole stover. While we did not see significant impacts to throughput, this was due to moisture failures of the first stage grinder in each system dominating failures and downtime. The operating cost savings of reduced grinding energy savings in the second stage hammer mills alone was high enough to offset the added capital cost of the air classifier and extra grinding line.

09 BIOMASS FUELS↗

DOE OSTI2023

Protein Extraction, Precipitation, and Recovery from Chlorella sorokiniana Using Mechanochemical Methods

Protein extraction, precipitation, and recovery methods were evaluated by this study using a green alga—Chlorella sorokiniana. A mechanochemical cell disruption process was applied to facilitate protein extraction from microalgal biomass. Optimization of the mechanochemical process resulted in milling conditions that achieved a protein extraction of 52.7 ± 6.45%. The consequent acid precipitation method was optimized to recover 98.7% of proteins from the microalgal slurry. The measured protein content of the protein isolate was 41.4% w/w. These results indicate that the precipitation method is successful at recovering the extracted proteins in the algal slurry; however, the removal of non-protein solids during centrifugation and pH adjustment is not complete. The energy balance analysis elucidated that the energy demand of the protein extraction and recovery operation, at 0.83 MJ/kg dry algal biomass, is much lower than previous studies using high-pressure homogenization and membrane filtration. This study concludes that mechanochemical protein extraction and recovery is an effective, low-energy processing method, which could be used by algal biorefineries to prepare algal proteins for value-added chemical production as well as to make algal carbohydrates and lipids in the residual biomass more accessible for biofuel production.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2023

Impact of Anatomical Fractionation of Corn Stover on Hammer Mill Throughput and Energy Consumption

ash content↗

DOE OSTI2024

Low Field NMR Relaxometry Characterization of Water Adsorption in Corn Stover Anatomical Fractions

Low magnetic field 2 MHz NMR relaxometry is applied to measure water adsorption processes of intact corn stover anatomical fractions. Comparison with high magnetic field 250 MHz relaxometry of milled corn stover fractions as a function of water activity, i.e., relative humidity, provides insight into the microstructural changes of the biomass and varying water molecular dynamics during adsorption. As a result, the data presented establish a basis for low field portable NMR of biomass in situ in field and processing environments.

09 BIOMASS FUELS↗

DOE OSTI2023

Coal-based Bricks & Blocks (CBBs): Process Development to Prototype Fabrication Coupled with Techno-Economic Analysis and Market Survey

The decline of coal use for energy production provides an abundance of local feedstock for new innovative uses and value-added products. Expanding the U.S. coal-value chain to manufacture high-value carbon products can strengthen the nation’s energy and mineral security, enhance the U.S. national defense security, increase the United States’ economic prosperity, while achieving U.S. environmental objectives. The primary project goal is a relatively light-weight composite product with superior (or comparable) compressive strength. Both virgin and, where available, post-consumer recycled thermoplastic versions are tested for each thermoplastic species. A useful attribute of thermoplastics as binders is that they can be heated to their melting point, cooled, and reheated again without significant degradation. A key advantage of thermoset CBBs is that they require only mixing and molding. CBB advantages include low cost, availability, binding ability and processability. Coal-based bricks and blocks (CBBs) weigh about 50% less than clay bricks and can be manufactured with an interlocking design to promote ease of use for the novice builder. CBB formulation is evaluated according to a design-of-experiments (DoE) approach. DoE variables are a) relative weight fractions of binder, b) relative proportions of large versus small (milled) anthracite size fractions, and c) additive percentage. Fabrication methods include hot-press molding and extrusion, the later being the most commercially viable. CBBs are tested for compressive strength, modulus of rupture (by flexure test) and water absorption per ASTM C67, with density determined by the Archimedes drainage method. Fractured interfaces are examined by SEM (Scanning Electron Microscopy) to resolve fracture dynamics and interior microstructure uniformity. Differential scanning calorimetry (DSC) is used to compare plastic transition temperatures i.e., glass and melting temperatures to contrast virgin with post-consumer recycled thermoplastics and optimize their usage. These results are used in the DoE analysis to identify the binder and relative weight percentages for optimum strength, density, and porosity. Overall, CBBs possess strength comparable to clay-based bricks but are non-permeable and hydrophobic, and hence resistant to degradation by freeze-fracturing, corrosion, and efflorescence. The strongest composites have been made with the following thermoplastic binders (in order of strength): thermoset, high-density polyethylene crosslink resin, high-density polyethylene, nylon 6/6, and polypropylene. Results from a techno-economic analysis TEA show economy of scale for CBBs by modularization and reveal the binder as the cost driver for material costs. Ideally, the incorporation of post-consumer recycled thermoplastic will decrease material acquisition costs and increase product sustainability. Notably, CBBs do not require the high temperature calcination needed to produce cement, nor do they require firing in the 1600-2400 °F range for three days using natural gas, as do clay brick equivalents. Instead, CBBs are heated to a modest <600 °F according to the melt flow index of the thermoplastic binder. Existing anthracite mines can be expanded to produce CBBs to reduce aggregate transportation costs and emissions that exist for clay bricks. TEA reflects this reduced energy cost while a comparative CO2 emission analysis quantifies the reduced environmental footprint. The market survey identifies several commercialization opportunities, dependent upon the brick classification.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2023

Coal-based Bricks & Blocks (CBBs): Process Development to Prototype Fabrication Coupled with Techno-Economic Analysis and Market Survey

Coal-based bricks and blocks (CBBs) were formulated using anthracite and thermoplastic binder. Lab scale test composites were formed by hot-press molding and commercial extrusion for test articles and for a full-scale prototype. Formulations and test matrices followed a systematic experimental design to examine the effects of and interactions among three primary independent variables: a) thermoplastic type, b) weight fractions of binder relative to the total anthracite weight, and c) relative proportions of large versus small (milled) anthracite size fractions. Technical performance metrics include compressive strength, modulus, porosity/permeability and density. These DoE studies establish composition-property relations and identify the best combination for any desired property of interest – in particular, strength. Based on CBB composition and fabrication process, validated against technical performance metrics, a techno-economic analysis was constructed which incorporated a process flow model, engineering design (with scaling), and calculated capital plus operating costs. Based on measured property metrics and estimated process economics and a projected price by TEA (techno-economic analysis), building and construction target markets were identified by a market survey assessment. With known cost, price, performance metrics and competitive advantages for CBBs matched with commercial applications/uses, a technical gap analysis was performed to identify further development required for scale-up and commercialization.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2023

Semihard magnetic properties of TiFe 2.5 iron-rich Laves phase and the effect of 4d- and 5d-element-substitutions for Ti

Rare-earth-free compounds exhibiting modest intrinsic hard magnetic properties may still yield viable permanent magnets if their constituent elements are abundant and inexpensive, and the properties are at least comparable to those of the hard ferrites. In this study, one such compound, the off-stoichiometric TiFe 2.5 Laves phase with the hexagonal C14 crystal structure, was found to exhibit – in addition to the already known room-temperature ferromagnetism – a uniaxial, albeit weak, magnetic anisotropy. With a Curie temperature of 422 K, saturation magnetization of 55.3 Am 2 /kg and magnetic hardness parameter of 0.97 this semihard compound is just below the threshold for being of interest for the development into permanent magnets. Replacing a small fraction of Ti with the 4d Nb and Mo or with the 5d Ta or W increases the anisotropy field, but only below room temperature. Replacing Ti with Zr or Hf increases the Curie temperature and leads to a spin reorientation below 200 K. All these substitutions, as well as combined (Zr,W) and (Nb,W) substitutions, fail to improve the room-temperature intrinsic hard magnetic properties of the Fe-rich Laves phase. Furthermore, an attempt to develop a room-temperature coercivity through high-energy ball-milling yielded a value of 0.026 T, an unusually small 2.9% fraction of the anisotropy field. Here, defects inherent in the C14 crystal lattice may be responsible for the underperformance.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Leading order track functions in a hot and dense QGP

We study the modifications to the fragmentation pattern of partons into charged particles in the presence of a hot and dense quark gluon plasma. To this end, we analyze the perturbative renormalization group equations of the track functions, which describe the energy fraction carried by charged hadrons. Focusing on pure Yang-Mills theory, we compute the lowest-order moments of the medium-modified track functions, which are found to be sensitive to the reduced phase space for emissions in the medium and to energy loss. We use the extracted moments to calculate the energy energy correlator (EEC) on tracks in the collinear limit. The EEC on medium-evolved tracks does not differ qualitatively from the EEC on vacuum tracks despite being sensitive to the color decoherence transition and suppressing the distribution due to quenching, as seen in other jet observables. Published by the American Physical Society 2024

Barata, João (ORCID:0000000342864555)↗

DOE OSTI2024

Nanostructured Alumina Forming Austenitic Alloy (NAFA) Production Using Mechanical Alloying and High-Temperature Consolidation

Alumina-forming austenitic (AFA) alloys are a promising class of nuclear materials because of their high-temperature oxidation/corrosion resistance and mechanical properties. Unfortunately, these alloys are limited in use for core material applications, and they are specifically limited for use as nuclear fuel cladding because of their high Ni-transmutation and helium generation rate in-service. Improving these alloys through a fine dispersion of oxide precipitates and thus increasing the effective irradiation sink strength of the alloy system may mitigate many of the degradation phenomena expected during alloy deployment. These phenomena include high-temperature helium embrittlement and cavity swelling for lead-cooled fast reactor applications. This work effort uses combination of conventional and advanced manufacturing approaches are being used to fabricate nanostructured AFA (NAFA) materials. As the first objective of this initiative, a conventional AFA was modified using mechanical alloying and extrusion to alter the precipitation characteristics to include a fine dispersion of nanoscale oxides intended to serve as traps for irradiation-induced point defects and transmuted He within the lattice. This analysis compared the efficacy of the conventional mechanical alloying and extrusion approach with the unalloyed AFA consolidated approach using hot isostatic pressing (HIP). It was found that, although the mechanical alloying approach is successful in producing a fine distribution of oxides within the first nanostructured AFA (NAFA-1), the distribution is heterogeneous because of the mild milling parameters used to prevent cold welding of powder to the spherical milling media. The additional dispersion of oxides, coupled with a higher volume fraction of other secondary phases in the NAFA-1, produces higher alloy strengths that range up to 600°C in comparison to the unalloyed HIP AFA, thus exceeding the operating temperature of lead-cooled fast reactors. However, the strength of the NAFA-1 is lower than that of the HIP AFA at 800°C, which is presumed to be a function of increased secondary phases from the nonoptimized AFA chemistry. Future work is planned on a newly procured NAFA-2 chemistry that is more suitable for advanced reactor applications exploring new manufacturing routes.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Characterization of ceramic fuel powder packing fractions to support INFLUX

Triply periodic minimal surface (TPMS)-based structures show marked potential in novel nuclear reactor fuel designs, as their high surface area-to-volume ratio increases the efficiency of heat transfer out of the fuel, enabling safer, more innovative reactor designs. This milestone report addresses the role of dUO 2 powder processing route on the fill behavior of TPMS-based cladding shells to understand and advance the feasibility of manufacturing TPMS-based nuclear fuel forms. dUO 2 powder was processed through either a dry granulation route, varying consolidation pressure, or through milling, varying milling time, milling method and milled size distribution. The lowest tapped bulk densities (TBD), but best powder flowabilities, were obtained when testing unprocessed dUO 2 powder which was prone to self-agglomeration and formed low-density spheroids. The highest TBD and lowest flowabilities were obtained when using powder produced by hammer-milling dUO 2 powder to pass through a 200-mesh sieve, which led to particles with angular morphologies. Powder produced by dry granulation exhibited TBD that varied according to the consolidation pressure used to form the initial pellets and exhibited improved flowabilities when compared to hammer-milled material. Because of the large span of granule sizes formed as well as the irregular shape associated with the granules, a packing fraction of 0.69 was achieved, exceeding the analytical solution for random close packing of mono-sized spheres. TPMS polymer shells were loaded with unprocessed, granulated, and hammer-milled dUO 2 powders, and their qualitative packing behaviors were analyzed using x-ray computed tomography (xCT). TBDs calculated after loading TPMS polymer shells were 10-20% lower when compared to tapped bulk density measurements taken in a glass graduated cylinder, indicating a non-trivial impact on the tapped bulk density of either the TPMS channel size, TPMS channel surface material, powder cohesiveness, or a combination of the two parameters. A metallic zircaloy-4 TPMS shell will be loaded with hammer-milled dUO 2 powder upon receipt of the shell from Oak Ridge National Laboratory (ORNL) and shipped to Idaho National Labs (INL) for subsequent hot isostatic pressing (HIP) densification experiments.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2023

Search for leptoquarks decaying into the bτ final state in pp collisions at $\sqrt{\textrm{s}}$ = 13 TeV with the ATLAS detector

A search for leptoquarks decaying into the $bτ$ final state is performed using Run 2 proton-proton collision data from the Large Hadron Collider, corresponding to an integrated luminosity of 139 fb —1 at $\sqrt{\textrm{s}}$ = 13 TeV recorded by the ATLAS detector. The benchmark models considered in this search are vector leptoquarks with electric charge of 2/3e and scalar leptoquarks with an electric charge of 4/3e. No significant excess above the Standard Model prediction is observed, and 95% confidence level upper limits are set on the cross-section times branching fraction of leptoquarks decaying into bτ. For the vector leptoquark production two models are considered: the Yang-Mills and Minimal coupling models. In the Yang-Mills (Minimal coupling) scenario, vector leptoquarks with a mass below 1.58 (1.35) TeV are excluded for a gauge coupling of 1.0 and below 2.05 (1.99) TeV for a gauge coupling of 2.5. In the case of scalar leptoquarks, masses below 1.28 (1.53) TeV are excluded for a Yukawa coupling of 1.0 (2.5). Finally, an interpretation of the results with minimal model dependence is performed for each of the signal region categories, and limits on the visible cross-section for beyond the Standard Model processes are provided.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2024

Herbaceous Feedstock 2022 State of Technology Report

The U.S. Department of Energy promotes production of advanced liquid transportation fuels from lignocellulosic biomass by funding fundamental and applied research that advances the state of technology (SOT). As part of its involvement in this mission, Idaho National Laboratory completes an annual SOT report for nth-plant and 1st-plant herbaceous biomass feedstock logistics. The purpose of the SOT is to provide the status of feedstock supply system technology development for herbaceous biomass to biofuels relative to technical targets and cost goals from specific design cases, based on data and experimental results. Although conventional feedstock supply systems form the backbone of the emerging biofuels industry, they have limitations that restrict widespread implementation on a national scale. To meet the demands of the future industry, the feedstock supply system must shift from the conventional system to what has been termed “advanced” supply systems. In advanced designs, a distributed network of aggregation and processing centers, termed “depots,” are employed near the points of biomass production (i.e., the field or forest) to reduce feedstock variability and produce feedstocks of a uniform format, moving toward biomass commoditization. The 2022 Herbaceous SOT is part of a vision of achieving an implemented advanced feedstock supply system, which produces a stable, tradable commodity at the decentralized distributed depot. It utilizes feedstock fractionation by incorporating technologies that can separate the biomass into its anatomical fractions (leaves, husks, stems and cobs) to reduce impurities and produce fractions that satisfy downstream quality considerations. By using a series of air classification steps, this strategy can reduce the extrinsic ash in corn stover and produce enriched tissue fractions that can be blended to a conversion specification or converted individually in optimized biochemical conversion campaigns. Additionally, a majority of the leaves (which do not meet the quality specification) are separated out early and can be supplied to alternate markets. The 2022 Herbaceous SOT incorporates an advanced biomass fractionation and processing system to produce pellets enriched tissues from three-pass corn stover. The resulting enriched pellets are delivered to the biorefinery individually where they can be blended to a specification or converted in campaigns where the conditions are optimized for each tissue. Unused fractions can be sent to a a midstream market or to a different conversion process that is better suited to their properties to offset the cost of the delivered feedstock. The main benefits from the proposed system can be summarized as: (1) $6.86/dry ton (2016$) lower cost for the air classification due to elimination of the requirement to discard the high ash lights fraction; (2) $1.56/dry ton lower delivered cost by selling the unsuitable leaf fraction into the feed market as a midstream co-product (assuming a selling price that is 11% higher than their cost of production); (3) 0.98% increase in carbohydrate content (from 60.16% to 61.14%); and (4) 0.97% decrease in ash content (from 6.00% to 5.03%) compared to the 2021 Herbaceous SOT. Overall, the 2022 nth-plant Herbaceous SOT predicts a modeled delivered feedstock cost of $78.64/dry ton (2016$) if it is assumed that the enriched leaf fraction is sold at its production cost; this is a slight increase of $0.43/dry ton increase from the 2021 Herbaceous SOT nth-Supply case cost. The increased cost derived from a $0.38/dry ton increase in transportation and handling cost to procure more biomass (to replace the enriched leaf fraction that was not delivered to the biorefinery. The total preprocessing cost was $0.27/dry ton higher than the 2021 result because of updates to energy consumption, purchasing price and dry matter loss data for the rotary shear ($3.00/dry ton increase) and the pelleting mill ($4.52/dry ton increase). The data utilized were generated in pilot-scale tests in the Biomass Feedstock National User Facility (BFNUF) at INL and at Forest Concepts, including tests for rotary shear and pelleting of the air classified fractions. A greenhouse gas emissions analysis was performed by Argonne National Laboratory using the most up to date version of the Greenhouse Gases, Regulated Emissions, and Energy use in Transportation model (GREET®). The analysis showed an increase of 17.34 kg CO2e/dry ton from the 2021 SOT (67.71 kg CO2e/ton in the 2021 Herbaceous SOT to 85.05 kg CO2e/ton in the 2022 Herbaceous SOT). The net increase is primarily attributed to increased energy consumption in pelleting mill.

09 BIOMASS FUELS↗

DOE OSTI2024

Lignin molecular weights of Populus trichocarpa residues after CELF pretreatment

Here we present a dataset of molecular weights of lignin from a woody energy crop (Populus trichocarpa) residues after a series of co-solvent enhanced lignocellulosic fractionation (CELF) pretreatment. The natural poplar variant GW-9947 from the Center for Bioenergy Innovation (CBI) was used. The poplar was knife milled and passed through a 1 mm sieve and CELF pretreatment was performed in a Parr autoclave reactor with 7.5 wt % solids loading, 0.5 wt% H2SO4 as catalyst at 150°C with various time. Tetrahydrofuran was added in a 1:1 mass ratio with water as the pretreatment solvent. Lignin was isolated from the pretreated samples after ball-milling in a porcelain jar with ceramic balls via Retsch PM 200 at 580 rpm for 2.5 h followed by enzymatic hydrolysis in acetate buffer (pH 4.8, 50 °C) for 48 h. The solid residue was isolated by centrifugation and hydrolyzed again with freshly added buffer and enzymes for another 48 h. After filtration, the solid residue was extracted twice with 96% (v/v) 1,4-dioxane/water mixture at room temperature overnight. The extracts were combined, rotary evaporated, and freeze-dried to recover lignin. The lignin samples were then derivatized in an acetic anhydride/pyridine (1:1, v/v) mixture and stirred at room temperature for 24 h. Ethanol was added to the reaction mixture, left for 30 min and then removed with a rotary evaporator. The addition and removal of ethanol was repeated at least 3 times until all traces of acetic acid were removed. Acetylated lignin samples were then dissolved in tetrahydrofuran (THF) at a concentration of 1.0 mg/mL. The molecular weight of acetylated lignin was measured by a gel permeation chromatography (GPC) on a PSS-Polymer Standards Service (Warwick, RI, USA) GPC SECurity 1200 system featuring Agilent HPLC 1200 components equipped with four Waters Styragel columns (HR1, HR2, HR4 and HR6) and an UV detector (270 nm). Tetrahydrofuran was used as the mobile phase and flow rate was 0.3 mL/min. The Polymer Standards Service WinGPC Unity software (Build 6807) was used for data processing for all the samples. The data provides information about the effects of CELF pretreatment time at 150 ºC on lignin molecular weights.

09 BIOMASS FUELS↗

DOE OSTI2024

Two-dimensional heteronuclear single quantum coherence (HSQC) NMR spectra of lignin isolated from Populus trichocarpa residues after CELF pretreatment and CBP fermentation

Here we present a curated dataset of a series of two-dimensional heteronuclear single quantum coherence (HSQC) nuclear magnetic resonance (NMR) spectra of lignin isolated from a woody energy crop (Populus trichocarpa) residues after co-solvent enhanced lignocellulosic fractionation (CELF) pretreatment and consolidated bioprocessing (CBP) process. The natural poplar variant GW-9947 from the Center for Bioenergy Innovation (CBI) was used. The poplar was knife milled and passed through a 1 mm sieve. The CELF pretreatment was performed in a Parr autoclave reactor with 7.5 wt % solids loading, 0.5 wt% H2SO4 as catalyst at 150°C with 15, 25 and 30 minutes, respectively. Tetrahydrofuran was added in a 1:1 mass ratio with water as the pretreatment solvent. The residues from CELF pretreatment were then subjected to CBP using the bacterium C. thermocellum DSM 1313. CBP fermentations were performed at 60 °C in a shaker at 50 grams/L solids loadings. Lignin was isolated from the pretreated samples after ball-milling in a porcelain jar with ceramic balls via Retsch PM 200 at 580 rpm for 2.5 h followed by enzymatic hydrolysis in acetate buffer (pH 4.8, 50 °C) for 48 h. The lignin samples were characterized using 13C–1H HSQC experiments which were performed in a Bruker Avance III HD 500 MHz NMR spectrometer operating at a frequency of 125.12 MHz for the 13C nucleus. A standard Bruker pulse sequence was used on a Prodigy platform cryoprobe. The dry lignin samples were dissolved in deuterated dimethylsulfoxide for HSQC experiments. The spectra were acquired under the following acquisition conditions: 210 ppm spectral width in F1 (13C) dimension with 256 data points and 11 ppm spectral width in F2 (1H) dimension with 1024 data points, a 90° pulse, a one bond C–H coupling constant of 145 Hz, a 1.0 s pulse delay, and 64 scans. All the data was processed using the TopSpin 3.6 software (Bruker BioSpin). The NMR spectra provides structural characteristics information about lignin remaining in solids after CELF (150 °C with 15, 25 and 30 minutes) process and C. thermocellum CBP.

Lignin structure, HSQC, poplar, CELF, CBP, CBI↗

DOE OSTI2024

Lignin content of Populus trichocarpa residues after CELF pretreatment and CBP fermentation

Here we present a dataset of lignin content from a woody energy crop (Populus trichocarpa) residues after a series of co-solvent enhanced lignocellulosic fractionation (CELF) pretreatment and consolidated bioprocessing (CBP) process. The natural poplar variant GW-9947 from the Center for Bioenergy Innovation (CBI) was used. The poplar was knife milled and passed through a 1 mm sieve and CELF pretreatment was performed in a Parr autoclave reactor with 7.5 wt % solids loading, 0.5 wt% H2SO4 as catalyst at 150°C with 5, 15, 25 and 30 minutes, respectively. Tetrahydrofuran was added in a 1:1 mass ratio with water as the pretreatment solvent. The residues from CELF pretreatment were then subjected to CBP using the bacterium C. thermocellum DSM 1313. CBP fermentations were performed at 60 °C in a shaker at 50, 75, and 100 grams/L solids loadings. The Klason lignin was measured using a two-step acid hydrolysis process. In brief, the poplar samples were first hydrolyzed by 72 wt% sulfuric acid at 30 oC for an hour. The hydrolysates were then diluted to 4 wt% sulfuric acid using deionized water and subsequently autoclaved at 121 oC for 1 h. Upon the completion of the two-step hydrolysis, the resulting solution was cooled to room temperature and the precipitate was then filtered through a G8 glass fiber filter through a crucible, dried at oven for overnight, and weighed to get the Klason lignin content. The lignin data provides information about lignin content changes after CELF and C. thermocellum CBP process.

Lignin Populus trichocarpa CELF pretreatment CBP f↗

DOE OSTI2026

Observations of Nocturnal Sulfuric Acid Formation in Pittsburgh, PA

Measurements of sulfuric acid (H 2 SO 4 ) and sulfur trioxide (SO 3 ) were conducted in Pittsburgh, Pennsylvania, during field campaigns in Fall 2023 and Fall 2024. These measurements identified nocturnal concentrations of H 2 SO 4 comparable to those of daytime values. Nocturnal H 2 SO 4 concentrations were observed to increase by 5 × 10 5 to 5 × 10 7 molecules cm –3 above background on 16 of the 31 measurement nights. The median peak concentration during events was 6.5 × 10 6 molecules cm –3 , with a maximum of 1.0 × 10 8 molecules cm –3 , exceeding previously reported nighttime concentrations. Increases in H 2 SO 4 concentrations were positively correlated with the anomalously high SO 3 concentrations and condensation sink rates, indicating that the formation of H 2 SO 4 increased to overcome the loss rates to particles. Increases in particulate mass and the mass fraction of metals commonly emitted from coal combustion and steel production were also observed. The air masses were traced back to the southeast of Pittsburgh, a region home to a steel mill, coke plant, and a steel processing plant. The observations indicate a previously unrecognized nighttime formation pathway for H 2 SO 4 , potentially from heterogeneous catalysis with metal or black carbon, originating from steel and coke plant emissions. Further measurements are needed to identify key compounds and chemical processes driving these increases in nocturnal H 2 SO 4 concentrations.

aerosols↗

DOE OSTI2023

Effects of Ball Milling on the Electrochemical Capacity and Interfacial Stability of Li 2 MnO 3 Cathode Materials

The cycling mechanism of Li 2 MnO 3 cathode materials synthesized by conventional solid-state methods at high temperatures (800-900 °C) has been intensively investigated. Previous studies showed that CO 2 and O 2 gas evolution accounts for most of the charge capacity, followed by some Mn reduction during discharge. In this work, we analyze the effects of ball milling on the structure, surface contaminant, and electrochemical capacity of Li 2 MnO 3 cathode material, with or without a graphitic fluoride (C-F) additive. At the same time, C-F is added to form a protective coating layer that reduces unwanted reactions with the electrolyte during later electrochemical cycling. We find that the C-F ball-milled material shows Li 2 MnO 3 /LiMnO 2 composite phases, while the purely ball-milled material shows a single Li 2 MnO 3 phase. Furthermore, we characterize surface species and gas evolution during the first cycle, which reveals the decomposition of Li 2 CO 3 and the carbonate electrolyte during the first charge, especially during the high potential region (>4.4 V), and the electrochemical reduction of only a small fraction of the evolved gas on the first discharge (<2.75 V). The appearance further demonstrates the repetitive nature of this process during charge and disappearance during discharge of Mn 2p 3/2 X-ray photoelectron spectroscopy (XPS) spectra signals during the first two cycles. These processes result in first discharge specific capacities of only 155 and 170 mAh/g after first charge specific capacities of 210 and 320 mAh/g for the pure ball-milled and ball-milled with C-F materials, respectively. These studies demonstrate the interfacial instability introduced by ball milling. However, the electrochemical capacity is significantly increased, necessitating further investigation to determine whether ball milling can activate Mn-containing cathode materials.

25 ENERGY STORAGE↗