A Simple Proposition for Improving Industrial Hygiene Air Sampling Methods
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47 OTHER INSTRUMENTATION↗
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Fast Extraction and Characterization of Fundamental Frequency Events from a Large PMU Dataset using Big Data Analytics
A novel method for fast extraction of fundamental frequency events (FFE) based on measurements of frequency and rate of change of frequency by Phasor Measurement Units (PMU) is introduced. The method is designed to work with exceptionally large historical PMU datasets. Statistical analysis was used to extract the features and train Random Forest and Catboost classifiers. The method is capable of fast extraction of FFE from a historical dataset containing measurements from hundreds of PMUs captured over multiple years. The reported accuracy of the best algorithm for classification expressed as Area Under the receiver operating Characteristic curve reaches 0.98, which was obtained in out-of-sample evaluations on 109 system-wide events over 2 years observed at 43 PMUs. Then Minimum Volume Enclosing Ellipsoid Algorithm was used to further analyze the events. 93.72% events were correctly characterized, where average duration of the event as seen by the PMU was 9.93 sec.
Baembitov, Rashid↗
The impact of mineral reactive surface area variation on simulated mineral reactions and reaction rates
Reactive transport modeling is an essential tool to simulate complex geochemical reactions in porous media that can impact formation properties including porosity and permeability. However, simulating these reactions is challenging due to uncertainties in model parameters, particularly mineral surface areas. Imaging has emerged as a powerful means of estimating model parameters including porosity and mineral abundance, accessibility and accessible surface area. However, these parameters, particularly mineral accessible surface area, vary with image resolution. This work aims to enhance understanding of the impact of image resolution and other means of estimating mineral reactive surface area on simulated mineral reactions and reaction rates. Mineral surface areas calculated from images with resolutions of 0.34 μm and 5.71 μm were used to simulate mineral reactions in the context of geologic CO 2 sequestration in the Paluxy formation at the continuum scale. Additional simulations were carried out using BET surface areas collected from the literature and geometric surface areas. Simulations were run for 7300 days and mineral volume fractions and effluent ion concentrations tracked and compared. Variations in mineral surface areas measured from images are within 1 order of magnitude and yield similar simulation results, indicating the impact of image resolution on simulated reactions and reaction rates is minimum for the resolutions and sample considered. In comparison, surface areas obtained from BET and geometric approaches are 1–4 orders of magnitude higher than image-obtained surface areas and result in greater simulated reaction rates and extents. Minerals with high reaction rates (calcite and siderite) are most impacted by surface area values at short times where simulated mineral volume fractions at longer times agree relatively well, even for simulations with several orders of magnitude variation in surface area. Phases with lower reaction rates, such as K-feldspar and muscovite, are predominantly impacted over longer times where variations in surface areas impact reaction extents and porosity evolution. Overall, variations in surface areas due to image resolution are small and result in little variation in simulated reactions and reaction rates while there are significant variations in simulation results when other surface area estimates are used. These variations, however, depend on the reactivity of the mineral phase where surface areas of fast-reacting phases largely impact simulations at short (hours to days) timescales and surface areas of slower-reactive phases impact longer term simulations (years).
58 GEOSCIENCES↗
Mechanical Characterization of High-Temperature Carbon Fiber-Polyphenylene Sulfide Composites for Large Area Extrusion Deposition Additive Manufacturing
Additive manufacturing (AM) is evolving from rapid prototyping to production of structural components. The widespread application of AM demands a high level of mechanical performance from these components, and it is therefore essential to improve feedstock material in order to meet these mechanical expectations. However, compared to traditional manufacturing techniques, the mechanical properties of AM materials and their resulting components are not well understood. In this study, we investigated the processability, microstructure, and mechanical performance of twin-screw compounded short carbon fiber reinforced polyphenylene sulfide (PPS) pellets as a feedstock material for big area AM (BAAM). The performance of the AM components was compared to that of traditional processing methods, namely injection molding (IM) and extrusion-compression molding (ECM). It was found that the AM composites exhibited 118% lower tensile strength and 55% lower tensile modulus when compared to traditional injection molding composite specimens; however, AM composites exhibited comparable properties to ECM composites. This response was attributed to highly aligned fibers in IM and AM samples. However, the AM composites contained porosity (15.5% volume), which reduced their mechanical properties in comparison to ECM composites. Finally, the IM process showed the maximum amount of fiber attrition with minimum porosity (0.007% volume), while the ECM process exhibited the least fiber attrition with 4.3% volume porosity.
36 MATERIALS SCIENCE↗
Isotopic evidence for a young lunar magma ocean
Herein, mare basalt sources and ferroan anorthosite suite cumulates define a linear array on a 146 Sm/ 144 Nd versus 142 Nd/ 144 Nd isochron plot demonstrating these materials were derived from a common reservoir at 4336 +31 / –32 Ma. The minimum proportion of the Moon that was in isotopic equilibrium at this time is estimated to be 1-3% of its entire volume based on the geographic extent from which the analyzed samples were collected and the calculated depths from which the samples were derived. Scenarios in which large portions of the Moon were molten to depths of many hundreds of kilometers are required to produce the observed Sm-Nd isotopic equilibrium between the mantle and crustal rocks at 4.34 Ga. This is a consequence of the fact that limited heating of a solid Moon above the blocking temperature of the Sm-Nd isotopic system is insufficient to diffusively homogenize radiogenic Nd throughout the mantle and crust. There are three scenarios that might account for global-scale isotopic equilibrium on the Moon relatively late in Solar System history including: (1) Sm-Nd re-equilibration of a solid Moon resulting from widespread melting in response to mantle overturn or a very large impact, (2) early accretion of the Moon followed by delayed cooling due to the presence of an additional heat source that kept a large portion of the Moon molten until 4.34 Ga, or (3) late accretion of the Moon followed by rapid cooling of the magma ocean late in Solar System history. Neither density-driven overturn of the mantle, nor a large impact, are likely to homogenize the mantle and crust to the extent required by the Sm-Nd isochron. Likewise, secondary heating mechanisms, such as tidal heating or radioactive decay, are not efficient enough to keep the Moon molten to the depth of the mare basalt source regions for many tens to hundreds of millions of years. Instead, the age of equilibrium between such a compositionally diverse set of rocks, produced on a global scale, likely records the time of primordial solidification of the Moon from a magma ocean. This scenario accounts for both the petrogenetic characteristics of lunar rock suites, as well as their Sm-Nd isotopic systematics. It is supported by the preponderance of ~4.35 Ga ages obtained for other hypothetical magma ocean crystallization products, such as ferroan anorthosite suite rocks and K, REE, and P enriched cumulates that are thought to represent flotation cumulates of the magma ocean and the last vestiges of magma ocean solidification, respectively.
79 ASTRONOMY AND ASTROPHYSICS↗
Thin-film chemical expansion of ceria based solid solutions: laser vibrometry study
The chemical expansion of Pr 0.1 Ce 0.9 O 2-δ (PCO) and CeO 2-δ thin films is investigated in the temperature range between 600 °C and 800 °C by laser Doppler vibrometry (LDV). It enables non-contact determination of nanometer scale changes in film thickness at high temperatures. The present study is the first systematic and detailed investigation of chemical expansion of doped and undoped ceria thin films at temperatures above 650 °C. The thin films were deposited on yttria stabilized zirconia substrates (YSZ), operated as an electrochemical oxygen pump, to periodically adjust the oxygen activity in the films, leading to reversible expansion and contraction of the film. This further leads to stresses in the underlying YSZ substrates, accompanied by bending of the overall devices. Film thickness changes and sample bending are found to reach up to 10 and several hundred nanometers, respectively, at excitation frequencies from 0.1 to 10 Hz and applied voltages from 0–0.75 V for PCO and 0–1 V for ceria. At low frequencies, equilibrium conditions are approached. As a consequence maximum thin-film expansion of PCO is expected due to full reduction of the Pr ions. The lower detection limit for displacements is found to be in the subnanometer range. At 800 °C and an excitation frequency of 1 Hz, the LDV shows a remarkable resolution of 0.3 nm which allows, for example, the characterization of materials with small levels of expansion, such as undoped ceria at high oxygen partial pressure. As the correlation between film expansion and sample bending is obtained through this study, a dimensional change of a free body consisting of the same material can be calculated using the high resolution characteristics of this system. A minimum detectable dimensional change of 5 pm is estimated even under challenging high-temperature conditions at 800 °C opening up opportunities to investigate electro-chemo-mechanical phenomena heretofore impossible to investigate. The expansion data are correlated with previous results on the oxygen nonstoichiometry of PCO thin films, and a defect model for bulk ceria solid solutions is adopted to calculate the cation and anion radii changes in the constrained films during chemical expansion. The constrained films exhibit anisotropic volume expansion with displacements perpendicular to the substrate plane nearly double that of bulk samples. The PCO films used here generate high total displacements of several 100 nm’s with high reproducibility. Consequently, PCO films are identified to be a potential core component of high-temperature actuators. They benefit not only from high displacements at temperatures where most piezoelectric materials no longer operate while exhibiting, low voltage operation and low energy consumption.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Design and Characterization of an Extremely-Sensitive, Large-Volume Gamma-Ray Spectrometer for Environmental Samples
A large volume gamma spectrometer was designed and constructed to analyze foodstuffs and environmental samples having low radionuclide concentrations. This system uses eight 11-cm × 42.5-cm × 5.5-cm NaI(Tl) detectors, chosen due to their relatively high sensitivity and availability and arranged in an octagonal configuration. The sensitive volume of the system is ~28 cm in diameter and ~42 cm deep. Shielding consists of an 86-cm × 86-cm square, 64-cm-tall lead brick enclosure with 18-cm-thick lead walls lined by 0.3-cm-thick copper plates. An aluminum top was machined to suspend the detectors within this shield. The shielding reduces background counts by 72% at 100 keV and 42% at 1,000 keV. The positional variability in sensitivity of the well was determined by both simulation and experiment. A 2.1-L volume of nearly uniform sensitivity, varying less than 10%, exists in the well's center. Energy resolutions of 14.6% and 7.8% were measured for 241 Am and 137 Cs, respectively. Energy resolution shows a 0.2% variation for both 241 Am and 137 Cs as a function of position within all regions of the well’s central sensitive volume. Dead time was also determined to be less than 35% for all sources measured in the system, the largest of which had an activity of 1,760 kBq. Simulated results for various source geometries show higher counts for smaller samples, especially at lower energies due to less attenuation of low energy photons. In conclusion, minimum detectable activities were determined for all source energies used, less than 5.1 Bq kg -1 for reasonable background and sample counting times.
47 OTHER INSTRUMENTATION↗
Survey of Technologies to Meet PAG limits for Detection of Cesium-137 in Water
The goal of this report is to evaluate the process of adding a sorbent to the sampling process to preconcentrate Cs-137 and then analyze the sorbent to provide a rapid assessment of results to guide decisions on drinking water sources and the protection of the public. Multiple unit design variables were considered: sample configuration/geometry, sorbent efficiency, sample volume. Model simulations demonstrated through these unit design efficiencies that 10 L of sample volume processed through a sorbent provides nearly two orders of magnitude improvement in sample counting time to provide results to a decision maker than the current process. Over 60 publications and reports concerning Cs-137 and sorbents were evaluated. The key attributes were readiness of sorbent to be deployed in a mobile laboratory environment, and minimum sample preparation and conditioning. Examples of sorbents not considered further included nanomaterials, which have not been evaluated at a commercial scale and are limited in availability. The recommended sorbents for further consideration include: ferrocyanide salts, zeolite, and chemically modified granular activated carbon.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Advances in Resin Management Using 3R-Scan - 20154
The most important factor underlying optimal waste management is developing a clear picture of the radioactivity content of the waste and its impact on waste disposal cost. For over 35 years since the publishing of 10CFR61, waste characterization has relied on sampling the final waste product after formation. In the days following 10CFR61, the cost of final disposal was marginal with only a small impact on the overall costs. Constraints were added by provisions of the Low Level Waste Policy Act of 1985 leading to increasingly limited access to those disposal sites that remained available. In addition, Nuclear Regulatory Commission (NRC) pressure promoting waste volume reduction led to disposal costs inevitably rising. Despite this, characterization practices in monitoring of waste generation for activity content still center on the same dated processes. This results in a disposal classification on the basis of endpoint sampling without consideration of the homogeneity of the waste mixture. It can also disregard consideration of the representativeness of the single or small sample base. As a minimum effort, a formalized sampling program of a fixed grouping of waste streams can be implemented that could account for more than 95% of all of the activity carried in solid waste products. The sample results for each radionuclide could then be trended as time passes to develop reasonable scaling factors for difficult to measure radionuclides. This process, identified in NRC guidance, has been rigorously followed by a relatively small number of facilities. The trended scaling factors serve to improve accuracy by identifying anomalous results that could otherwise go undetected. Direct monitoring of the accumulation of activity in process streams generating solid radwaste, including demineralizers and filter streams, is a more precise approach. Nearly all of these streams are monitored by plant chemistry on a regular schedule to maintain water quality. This paper discusses viable options for developing the basis for characterization through process monitoring of the accumulation of activity at the point of generation. Special focus is on resin bed tracking and how process knowledge of these streams can be brought together to form a consistent and precise solid waste radioactivity inventory. Some of the specific points covered in this paper include the merger of the fission product release computer program, 3R-STAT, with the radwaste sample analysis computer program, SCAN4 to create 3R-SCAN, the importance of individual waste stream influences on the overall source term, and the use of historic sample data to develop scaling factors using an automated process. (authors)
12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
A PIPS + SrI 2 (Eu) detector for atmospheric radioxenon monitoring
The PIPS–SrI 2 (Eu) is a prototype atmospheric radioxenon detection system designed at Oregon State University in support of international efforts towards monitoring clandestine nuclear weapon testing activities. This detector aims to address some shortcomings found in currently deployed beta–gamma atmospheric radioxenon detection systems, such as lackluster energy resolution and memory effect, by employing modern detection materials and readout. The system uses a PIPSBox, a silicon-based gas cell, for electron detection, and a pair of ultrabright, D-shaped SrI 2 (Eu) scintillators coupled to silicon photomultipliers for photon detection. A custom eight-channel digital pulse processor equipped with a field programmable gate-array (FPGA) identifies electron–photon coincidences between the volumes in near real-time. Gas samples of the four radioxenon isotopes of interest were independently measured with the PIPS–SrI 2 (Eu) detection system to determine energy resolution and efficiency. Application of FPGA-based coincidence discrimination in near real-time reduced the ambient background count rate by 95.85 ± 0.04%. Using parameters from the Xenon International gas processing unit and assuming a blank sample and zero memory effect the minimum detectable concentrations (MDCs) for the isotopes were calculated to be 0.12 ± 0.03, 0.27 ± 0.05, 0.15 ± 0.02, and 1.00 ± 0.08 mBq/m 3 air for 131m Xe, 133 Xe, 133m Xe, and 135 Xe, respectively. These MDC estimates compare well with other radioxenon detection systems employed in the International Monitoring System (IMS) and indicate that the PIPS–SrI 2 (Eu) is in compliance with the Comprehensive Nuclear Test-Ban-Treaty Organization (CTBTO) sensitivity requirement of ≤ 1 mBq/m 3 for 133 Xe.
46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
Top Loading Helium Cryostat Integrated with High-Pressure Cell with Fast Remote Pressure Control (Final Report for SBIR Phase 1)
A large number of physical phenomena, such as superconductivity and quantum critical phenomena, often appear only at very low temperatures below 5 K. There is an immense interest to investigate these phenomena at high pressure as a means of tuning interatomic distances, and thus the interaction parameters controlling these phenomena, in a continuous and controlled fashion. The current P-T condition for neutron scattering experiments are limited to either relatively low pressures of about 2 GPa at temperatures below 5 K, or to relatively high temperatures at pressures or tens of GPa. The purpose of this research is to develop neutron sample environment instrumentation for reaching 10-20 GPa at 1-2K with rapid and reliable online pressure and temperature control (i.e. without having to interrupt the experiment). The ultimate goal of the project is to design an integrated fast-cooling low-temperature sample environment cryogenic system compatible with state of the art neutron diamond anvil cells suitable for single-crystal neutron scattering experiments for temperatures down to 2K and pressures of several tens of GPa. The integrated system will consist of top-loading Helium flow cryostat with in-situ sample alignment mechanisms, large-volume diamond anvil cells (DAC) made from novel superalloy Pascalloy and optimized for fast cooling and heating, and a compact remote pressure control mechanism for the DAC based on a novel concept of inflatable bellows integrated with a lever-arm based force amplifier. In Phase I, we have designed, manufactured, and tested prototypes of the novel compact force-amplified pneumatic pressure control mechanism for Neutron Diamond Anvil Cell (nDAC), which allows to use pneumatic bellows system for smooth remote pressure control in the nDAC inside a top-loading cryostat with bore size of 70 mm or larger. This allows significant minimum temperature decrease in remotely controlled nDAC from 5-10 K down to 2 K. We also studied mechanical properties of a novel non-magnetic superalloy Pascalloy with different heat-treatment conditions and preliminary results indicate that up to date this is probably the strongest and most suitable material for making more compact and lightweight cryogenic nDACs for neuron scattering experiments at extreme conditions, allowing much faster cooling and heating. Potential applications: The new developments will allow to create a wide range of compact Diamond Anvil Cells for neutron diffraction which can reach several tens of GPA pressure at 2-4 K while preserving accurate remote pressure control capabilities. The new concepts can be used for developing sample environment instrumentation outside the neutron scattering field. The new development have very strong potential for expanding experimental capabilities in materials sciences and have high commercialization potential. The proposed new cryogenic high-pressure system or any of its individual components will be in high demand not only in neutron scattering facilities, but also at synchrotron beamlines and other high-pressure research facilities around the world.
36 MATERIALS SCIENCE↗
Mafic explosive volcanism at Llaima Volcano: 3D x-ray microtomography reconstruction of pyroclasts to constrain shallow conduit processes
Abstract Mafic volcanic activity is dominated by effusive to mildly explosive eruptions. Plinian and ignimbrite-forming mafic eruptions, while rare, are also possible; however, the conditions that promote such explosivity are still being explored. Eruption style is determined by the ability of gas to escape as magma ascends, which tends to be easier in low-viscosity, mafic magmas. If magma permeability is sufficiently high to reduce bubble overpressure during ascent, volatiles may escape from the magma, inhibiting violent explosive activity. In contrast, if the permeability is sufficiently low to retain the gas phase within the magma during ascent, bubble overpressure may drive magma fragmentation. Rapid ascent may induce disequilibrium crystallization, increasing viscosity and affecting the bubble network with consequences for permeability, and hence, explosivity. To explore the conditions that promote strongly explosive mafic volcanism, we combine microlite textural analyses with synchrotron x-ray computed microtomography of 10 pyroclasts from the 12.6 ka mafic Curacautín Ignimbrite (Llaima Volcano, Chile). We quantify microlite crystal size distributions (CSD), microlite number densities, porosity, bubble interconnectivity, bubble number density, and geometrical properties of the porous media to investigate the role of magma degassing processes at mafic explosive eruptions. We use an analytical technique to estimate permeability and tortuosity by combing the Kozeny-Carman relationship, tortuosity factor, and pyroclast vesicle textures. The groundmass of our samples is composed of up to 44% plagioclase microlites, > 85% of which are < 10 µm in length. In addition, we identify two populations of vesicles in our samples: (1) a convoluted interconnected vesicle network produced by extensive coalescence of smaller vesicles (> 99% of pore volume), and (2) a population of very small and completely isolated vesicles (< 1% of porosity). Computed permeability ranges from 3.0 × 10 −13 to 6.3 × 10 −12 m 2 , which are lower than the similarly explosive mafic eruptions of Tarawera (1886; New Zealand) and Etna (112 BC; Italy). The combination of our CSDs, microlite number densities, and 3D vesicle textures evidence rapid ascent that induced high disequilibrium conditions, promoting rapid syn-eruptive crystallization of microlites within the shallow conduit. We interpret that microlite crystallization increased viscosity while simultaneously forcing bubbles to deform as they grew together, resulting in the permeable by highly tortuous network of vesicles. Using the bubble number densities for the isolated vesicles (0.1-3 −3 × 10 4 bubbles per mm 3 ), we obtain a minimum average decompression rate of 1.4 MPa/s. Despite the textural evidence that the Curacautín magma reached the percolation threshold, we propose that rapid ascent suppressed outgassing and increased bubble overpressures, leading to explosive fragmentation. Further, using the porosity and permeability of our samples, we estimated that a bubble overpressure > 5 MPa could have been sufficient to fragment the Curacautín magma. Other mafic explosive eruptions report similar disequilibrium conditions induced by rapid ascent rate, implying that syn-eruptive disequilibrium conditions may control the explosivity of mafic eruptions more generally.
Valdivia, Pedro↗
Benchmark of the Chlorine Worth Study Experiments in Support of Chlorine Nuclear Data Validation for Nuclear Criticality Safety
The Chlorine Worth Study (CWS) was a critical experiment to address an urgent need for thermal chlorine nuclear data validation in plutonium systems. This urgent need is tied directly to plutonium recycle and recovery operations in the plutonium facility at Los Alamos National Laboratory, where exceptionally conservative criticality safety limits are used because no credit is taken for the neutron capture by chlorine. The experiment used weapons-grade plutonium metal plates clad in stainless steel, known as the PANN (plutonium aluminum no nickel) ZPPR (zero power physics reactor) plates. The plutonium was reflected and moderated by high-density polyethylene and included combinations of polyvinyl chloride (PVC) and chlorinated polyvinyl chloride (CPVC) as absorbers. The experiment and benchmark included three configurations mimicking 30 g 239 Pu/L plutonium, 300 g 239 Pu/L plutonium, and 600 g 239 Pu/L plutonium in an aqueous chloride solution. Uncertainties in the benchmark included five broad categories: (1) criticality measurement, (2) mass and density, (3) dimensions, (4) material compositions, and (5) positioning. The largest contribution to the overall uncertainties for all three cases came from the material compositions, in particular the PVC and CPVC absorber compositions. A detailed model was created to be a near match (that is within expectations of transport code users) and a simplified model was created to minimize offset dimensions and expedite modeling for code validation. Sample calculations were completed in MCNP6.3 with ENDF/B-VIII.0 and ENDF/B-VII.1 nuclear data. For the detailed and simplified models, the average difference between the computed and experimental k eff was 951 pcm. CWS will serve as the key validation experiment for nuclear criticality safety in support of aqueous chloride operations. The sensitivity to the chlorine capture cross section is orders of magnitude greater than other existing benchmarks. The current limits, as defined by nuclear criticality safety, are 520 g Pu per batch, i.e. the minimum critical mass of the Pu solution infinitely reflected by water [Criticality Handbook: Volume II, (1969)]. This extremely conservative critical mass limit does not credit any neutron capture by chlorine (in particular neutron capture by 35 Cl) and greatly impedes the throughput required for current and future operations.
73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
Instrumentation and methods for efficient time-resolved X-ray crystallography of biomolecular systems with sub-10 ms time resolution
Time-resolved X-ray crystallography has great promise to illuminate structure–function relations and key steps of enzymatic reactions with atomic resolution. The dominant methods for chemically-initiated reactions require complex instrumentation at the X-ray beamline, significant effort to operate and maintain this instrumentation, and enormous numbers (∼10 5 –10 9 ) of crystals per time point. We describe instrumentation and methods that enable high-throughput time-resolved study of biomolecular systems using standard crystallography sample supports and mail-in X-ray data collection at standard high-throughput cryocrystallography synchrotron beamlines. The instrumentation allows rapid reaction initiation by mixing of crystals and substrate/ligand solution, rapid capture of structural states via thermal quenching with no pre-cooling perturbations, and yields time resolutions in the single-millisecond range, comparable to the best achieved by any non-photo-initiated method in both crystallography and cryo-electron microscopy. Our approach to reaction initiation has the advantages of simplicity, robustness, low cost, adaptability to diverse ligand solutions and small minimum volume requirements, making it well suited to routine laboratory use and to high-throughput screening. We report the detailed characterization of instrument performance, present structures of binding of N -acetylglucosamine to lysozyme at time points from 8 ms to 2 s determined using only one crystal per time point, and discuss additional improvements that will push time resolution toward 1 ms.
Indergaard, John A. (ORCID:000000022367699X)↗
Benchmarking image processing techniques for porosity measurement in polymer additive manufacturing: Review and experimental analysis
An image processing workflow is proposed for porosity measurement in polymer additive manufacturing. Various techniques, including global and local thresholding, region growing, and K-means clustering, were applied to microscopic images of carbon fiber reinforced acrylonitrile butadiene styrene (CF-ABS) and benchmarked for their ability to accurately measure porosity. Global methods included Otsu, minimum error, iterative, and entropy-based thresholding, while local methods included Niblack, Bernsen, Sauvola, and Bradley-Roth algorithms. Artificial uneven illumination was introduced to test local adaptive thresholds. Results showed significant differences in porosity values across methods. Otsu, region growing, and K-means clustering excelled under uniform illumination, while Sauvola and Bradley-Roth performed better with uneven illumination. Comparison with X-ray computed tomography (XCT) revealed slightly lower porosity values (2.55 %) than optimized methods (2.73–2.79 %) due to XCT's lower resolution excluding smaller pores. While XCT offers finer pore detection, it limits sample volume and underestimates porosity due to spatial variation. Validation using artificial grayscale images with 5 % porosity confirmed that Otsu, Bradley-Roth, region growing, and Sauvola algorithms produced accurate results. Although tested on a single material system, these methods can be adapted to others with optimization. In conclusion, given XCT's high computational and time costs, this study highlights suitable image processing techniques as cost-effective alternatives for porosity analysis in polymer composites.
Additive manufacturing↗
Estimating Soil Thermal Inertia Profiles From the Passive Equilibration of a Temperature Probe
Knowledge of the distribution of soil thermal properties is important for understanding subsurface hydrological and biogeochemical processes. This study describes and evaluates quick thermal profiling (QTP), a new measurement technique aimed at providing rapid, depth-resolved measurements of soil thermal inertia at numerous locations across the landscape. A cylindrical probe with temperature sensors at multiple depths is quickly inserted into the ground, and soil thermal inertia is estimated from how quickly the probe temperature equilibrates with the soil. To this end, a finite volume heat transfer model is used to generate temperature equilibration time series across combinations of controlling factors, and a gridded search inversion approach is applied to infer soil thermal inertia. Field tests in the Arctic indicate that QTP measurements have a minimum uncertainty of 0.14 J m −2 K −1 s −1/2 and covary with dual-probe heat pulse thermal analyzer measurements (concordance correlation coefficient = 0.56) with a root-mean-square error of 0.40 J m −2 K −1 s −1/2 . Besides demonstrating the value of QTP for estimating thermal inertia, this study identifies various sources of measurement uncertainty, particularly probe-soil contact resistance and frictional heating. Further, analysis of soil samples indicates that thermal inertia can be used to estimate thermal conductivity and dry bulk density in the studied area, although such inferences are highly site-specific. Overall, the QTP method holds promise to generate thermal inertia data products and to complement other characterization approaches for advancing understanding of soil properties across far more locations than is currently possible.
Lamb, J. R. [Lawrence Berkeley National Laboratory↗
NORTH DAKOTA CARBONSAFE PHASE III: SITE CHARACTERIZATION AND PERMITTING OF GEOLOGIC STORAGE OF CARBON DIOXIDE
The Energy & Environmental Research Center (EERC), in partnership with Minnkota Power Cooperative Inc. (Minnkota), SLB, and Computer Modelling Group Ltd. (CMG), supported wide-scale deployment of carbon capture and storage (CCS) as part of the U.S. Department of Energy (DOE) National Energy Technology Laboratory Carbon Storage Assurance Facility Enterprise (CarbonSAFE) Initiative Phase III. This phase included the acquisition, analysis, and development of information to fully characterize two storage complexes to demonstrate viable storage resources for commercial volumes of CO2 (defined by DOE as a minimum of 50 million tonnes [MMt] of CO2 within a 30-year period) (National Energy Technology Laboratory, 2024). Phase III also involved the preparation, submission, and approval of North Dakota underground injection control (UIC) Class VI storage facility permits (SFPs)—required precursors to applications for Class VI injection well permits. The presumed viability of commercial-scale CCS, situated adjacent to Minnkota’s Milton R. Young Station (MRYS), is validated by Minnkota’s continued pursuit of Project Tundra—an initiative to build the world’s largest lignite-based CCS project in central North Dakota (www.projecttundrand.com). Project Tundra comprises two scopes of work, Tundra Capture (installation of postcombustion CO2 capture at MRYS) and Tundra SGS (secure geologic storage). The efforts of North Dakota CarbonSAFE Phase III, Site Characterization and Permitting, supported Tundra SGS. Extensive site-specific characterization activities included a successful multimeasurement geophysical approach and drilling a stratigraphic test well (J-ROC 1, subsequently renamed Liberty-1) adjacent to MRYS. Core collection and analyses, downhole testing and fluid sampling, and geophysical logging were performed on J-ROC 1 and on a nearby stratigraphic test well (known as J-LOC 1), which was drilled, cored, and tested under a complementary project funded by the North Dakota Lignite Research Program. The injection tests performed on J-LOC 1 positively impacted the CarbonSAFE project, resulting in fewer proposed injection wells and significant construction, operations, and monitoring cost savings. The characterization data collected and analyses performed were integrated into geologic models, and successive numerical simulations were run to determine CO2 plume extent and subsurface pressure buildup associated with the planned CO2 injection rate of nearly 4 MMt per year. The latter doubles the CarbonSAFE Initiative goal with an estimated 100 MMt of CO2 stored in 20 years. Application of the U.S. Environmental Protection Agency’s (EPA’s) method for estimating the Class VI Rule area of review (AOR) to the overpressurized Broom Creek Formation inspired an alternative method of calculation, called risk-based AOR delineation. This peer-reviewed method was applied for the first time during the storage facility-permitting process. The two SFP applications submitted in 2021 successfully resulted in North Dakota Industrial Commission (NDIC) orders in 2022 authorizing the creation of the storage facility areas and amalgamation of pore space as well as establishing financial responsibility requirements. After approval of the SFPs, Minnkota filed in 2022 applications for permits to reenter the J-ROC 1 well and to drill two new wells—all with the intended purpose to become Class VI injection wells. To establish eligibility under the Internal Revenue Code for Section 45Q tax incentives, a monitoring, reporting, and verification (MRV) plan was prepared and submitted by Minnkota to EPA in 2022, resulting in the first such plan approved in North Dakota. Also in 2022, under the National Environmental Policy Act (NEPA), Minnkota prepared and submitted an environmental information volume (EIV) describing the proposed CCS project and associated potential environmental impacts. Based on the EIV, DOE determined that the proposed construction project required an environmental assessment, and Minnkota submitted the first draft in 2023 and a revised draft in 2024. Both submissions were followed by a public comment period. Subsequently, DOE issued a finding of no significant impact (FONSI) on September 13, 2024. A successful outreach program, strongly based in the production, presentation, and dissemination of informational material, fostered an environment to aid stakeholders in making informed decisions regarding the planned project. Opportunities for public input were provided at various steps along the way, including at county planning and zoning meetings, before and during the SFP administrative hearing, and during environmental assessment public comment periods. In addition, land/pore space owners and mineral owners had various points of contact, including granting access rights, securing pore space leasing, and mineral owner notifications. Based upon the successful storage facility permitting issued by NDIC, approval of the MRV plan by EPA, and receipt of a FONSI under the NEPA, Minnkota is continuing its pursuit of Project Tundra. In December 2023, the Office of Clean Energy Demonstrations under its Carbon Capture Demonstrations Projects Program announced funding for the capture system (Office of Clean Energy Demonstrations, 2023) and a proposal for CarbonSAFE Phase IV: Construction funding was submitted in March 2024 for the storage project. A go/no-go decision to proceed with construction and operations in the Broom Creek Formation is anticipated in 2024. References National Energy Technology Laboratory, CarbonSafe Initiative, https://netl.doe.gov/carbon-management/carbon-storage/carbonsafe (accessed August 2024). Office of Clean Energy Demonstrations, 2023, OCED selects three projects in CA, ND, and TX to reduce harmful carbon pollution, create new economic opportunities, and advance carbon reducing technologies, December, www.energy.gov/oced/articles/oced-selects-three-projects-ca-nd-and-tx-reduce-harmful-carbon-pollution-create-new (accessed August 2024).
Peck, Wesley↗
Depth and elevation of floodplain fine sediment along the East River near Crested Butte, Colorado measured in 2016 and 2017
The depth of floodplain fine sediment was measured at 1,601 points along the East River near Crested Butte, Colorado spanning a study reach approximately 800 m in length in 2016 and 2017. These depths are being used to estimate the volume of floodplain sediment present along the study reach, converted into mass of sediment using bulk density measurements, and finally used to estimate the mass of organic carbon stored in the floodplain based on elemental analysis of percent organic carbon content. Recorded depths include a minimum of 1 cm, a median of 56 cm, a maximum of 175 cm, and a mean with standard deviation of 61 ± 34 cm. This data include a csv file of the coordinates for each point in NAD 83 UTM zone 13, measured sediment depths, distance from the river channel active during 2015 measured using geographic information systems, the elevation of the floodplain surface derived from 0.5-m resolution lidar, and the elevation of the underlying gravel/bedrock surface, and in some cases the distance from the active channel measured in the field along the sampling transect. Also included is an ESRI ArcMap shapefile of the measurement points complete with the data listed above.
54 ENVIRONMENTAL SCIENCES↗