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DOE OSTI2024

DECOVALEX-2023: Task E Final Report

This is the Task E final report for DECOVALEX-2023. Task E is focused on understanding thermal, two-phase hydrological, and mechanical (TH2M) processes, especially related to predicting brine migration in the excavation damaged zone around a heated excavation in salt. Salt is attractive as a disposal medium for radioactive waste because it is self-healing and is essentially impermeable and essentially non-porous in the far field (away from excavations). Investigation of the short-term (days to years) near-field (centimeters to tens of meters) behavior of salt is important for radioactive waste disposal because this early period strongly controls the amount of brine in a salt repository. Brine leads to corrosion of waste forms and waste packages, and possible dissolution of radionuclides with brine transport being a potential transport vector to the accessible environment. The main test case used in Task E is the ongoing Brine Availability Test in Salt (BATS) heater test located underground at the Waste Isolation Pilot Plant (WIPP) near Carlsbad, New Mexico, USA. The Task was divided into a series of Steps. Step 0 was an introduction to processes in salt, that included matching historical unheated brine inflow data from boreholes at WIPP and matching temperature observations during BATS heater test 1a. Step 1 included validation of models against a thermo-poroelastic analytical solution relevant to heated boreholes in salt, and two-phase flow around an excavation in salt. Step 2 required all the individual components covered in steps 0 and 1 to come together to match observed brine inflow behavior during the BATS 1a heater test. There were a range of approaches from the teams, from mechanistic to prescriptive. Given the uncertainties in the problem, some teams used one- or two-dimensional models of the processes, while other teams included more geometrical complexity in three-dimensional models. The key learning points from Task E have been: • Heat conduction through salt typically requires non-linear thermal conductivity (as a function of temperature), but most models do a good job matching observations, given appropriate adjustments to the applied power and some thermocouple locations. • Thermal pressurization requires coupled thermal-hydrological-mechanical (THM) responses that consider the thermal expansion of the fluid and solid phases. • Initialization of two-phase flow models around a borehole or excavation in salt are more realistically represented as “wetting up”, rather than “drying down” (i.e., the initial state after excavation is mostly dry, rather than mostly wet). • The BATS 1a heater test includes a significant release of brine after the end of heating, which requires a large increase in permeability to recreate. Task E has been a great learning experience for all the teams involved, and feedback from the modeling teams has led to changes in the design of follow-on BATS experiments, which are now ongoing underground at WIPP. There was a balance throughout the task between freedom to model phenomena how each team saw fit, and prescriptiveness in problem design to bring the modeling teams closer together to allow attribution of smaller differences between models to different modeling choices. The modeling approaches seem to go through two phases: an early phase of discovery or testing, and a later phase of refinement and improvement. In future modeling efforts, different field data could be used (e.g., BATS 2) and more time should be included in the processes for teams to make multiple model refinement or even significant changes to their conceptual model or setup, based on lessons learned from the modeling exercise.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

NASA NTRS1987

Pressure probe study of the water relations of Phycomyces blakesleeanus sporangiophores

The physical characteristics which govern the water relations of the giant-celled sporangiophore of Phycomyces blakesleeanus were measured with the pressure probe technique and with nanoliter osmometry. These properties are important because they govern water uptake associated with cell growth and because they may influence expansion of the sporangiophore wall. Turgor pressure ranged from 1.1 to 6.6 bars (mean = 4.1 bars), and was the same for stage I and stage IV sporangiophores. Sporangiophore osmotic pressure averaged 11.5 bars. From the difference between cell osmotic pressure and turgor pressure, the average water potential of the sporangiophore was calculated to be about -7.4 bars. When sporangiophores were submerged under water, turgor remained nearly constant. We propose that the low cell turgor pressure is due to solutes in the cell wall solution, i.e., between the cuticle and the plasma membrane. Membrane hydraulic conductivity averaged 4.6 x 10(-6) cm s-1 bar-1, and was significantly greater in stage I sporangiophores than in stage IV sporangiophores. Contrary to previous reports, the sporangiophore is separated from the supporting mycelium by septa which prevent bulk volume flow between the two regions. The presence of a wall compartment between the cuticle and the plasma membrane results in anomalous osmosis during pressure clamp measurements. This behavior arises because of changes in solute concentration as water moves into or out of the wall compartment surrounding the sporangiophore. Theoretical analysis shows how the equations governing transient water flow are altered by the characteristics of the cell wall compartment.

NASA Discipline Number 40-30↗

DOE OSTI2024

Miniaturized Magnetoelastic Sensor System

This article describes the design, assembly, and implementation of a hand-held, magnetic-field-based sensor system that can be adapted for a variety of sensing applications. The miniaturized system is based on Chemical Identification by Magneto-Elastic Sensing (ChIMES) technology, which uses three concentric solenoid coils to wirelessly interrogate a sensor body comprised of a response material coupled to a magnetoelastic wire. The response material expands when it encounters a target, imposing mechanical stress on the wire and altering its magnetic permeability. The sensor bodies are passive, requiring no external power source, and they are small, measuring about 15 mm in length and 3.0 mm in diameter. Up to four sensor bodies can be configured as an evenly-spaced linear array. The sensor system operates by applying a low-frequency, current-stabilized, filtered triangle wave to a uniform-density excitation coil to switch the magnetic domains within the wire. Further, the responses from the sensors are picked up by a detection coil as stress-induced changes in the Faraday voltage, and the strong magnetic field induced by the excitation coil in the detection coil is nullified by a cancellation coil reverse-wound in series with the detection coil. The responses of the sensors in an array are separated in time by a linear gradient dc biasing coil. The sensors can be interrogated through metallic and nonmetallic barriers. The signals from the detection coil and the excitation coil are digitized by a pair of bipolar analog-to-digital converters (ADCs). A Raspberry Pi single-board computer (SBC) and associated software perform data acquisition and control all aspects of the sensor system hardware. The program allows the user to select the number of sensors in the array, the type of signal that is being collected, and the number of samples to take. The program also allows for signal processing of the sensor data, such as baseline correction. The program can differentiate sensor peaks from each other and calculate the magnitude of each sensor response with less than 1% error. The data are then displayed along with a graph of the signal.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

NASA NTRS2016

Additive Manufacturing, Design, Testing, and Fabrication: A Full Engineering Experience at JSC

I worked on several projects this term. While most projects involved additive manufacturing, I was also involved with two design projects, two testing projects, and a fabrication project. The primary mentor for these was Richard Hagen. Secondary mentors were Hai Nguyen, Khadijah Shariff, and fabrication training from James Brown. Overall, my experience at JSC has been successful and what I have learned will continue to help me in my engineering education and profession long after I leave. My 3D printing projects ranged from less than a 1 cubic centimeter to about 1 cubic foot and involved several printers using different printing technologies. It was exciting to become familiar with printing technologies such as industrial grade FDM (Fused Deposition Modeling), the relatively new SLA (Stereolithography), and PolyJet. My primary duty with the FDM printers was to model parts that came in from various sources to print effectively and efficiently. Using methods my mentor taught me and the Stratasys Insight software, I was able to minimize imperfections, hasten build time, improve strength for specific forces (tensile, shear, etc...), and reduce likelihood of a print-failure. Also using FDM, I learned how to repair a part after it was printed. This is done by using a special kind of glue that chemically melts the two faces of plastic parts together to form a fused interface. My first goal with SLA technology was to bring the printer back to operational readiness. In becoming familiar with the Pegasus SLA printer, I researched the leveling, laser settings, and different vats to hold liquid material. With this research, I was successfully able to bring the Pegasus back online and have successfully printed multiple sample parts as well as functional parts. My experience with PolyJet technology has been focused on an understanding of the abilities/limits, costs, and the maintenance for daily use. Still upcoming will be experience with using a composite printer that uses FDM technology to print plastic while laying an internal filament of Kevlar or carbon-fiber inside the printed material. It has been incredible being exposed to this range of technologies and I feel very fortunate to be ready for virtually any kind of printing technology I come across in the future. Design work played a part in my internship this term as well. Working with Hai Nguyen, I was able to design a set of testing tips and a test frame for use with an Arcjet. The testing tips will be made of several different materials that will possibly be used in the heat shield of the Orion space craft. These designs included technical drawings that were presented to the fabrication shop. The frame design was created from 80/20 (a popular brand of frame construction equipment) and included an order form with pricing for fabrication. An independent design was also done for the virtual reality lab. This design was to create a hand-controller based on a previous design. This final design was sent directly to a 3D printer without technical drawings. Overall, my design work has given me experience with using 80/20, helped improve my CAD (Computer Aided Design) proficiency, and increased my knowledge of how to set up technical drawings for fabrication. The final role I have played in this internship has been to assist with testing of the inflatable technology materials working Khadijah Shariff. I began the internship assisting with permeability testing with the initial plan to continue the testing independently after training. Unfortunately, the testing apparatus suffered a technical failure and had funding pulled which cancelled that portion of the project. Further testing with inflatable technology continued with tensile testing of various stitching methods. This testing took place over a two-days and concluded successfully. Final testing was to be more tensile testing but of straps used to connect various inflatable sections. Unfortunately, the needed grips for the tensile tests could not be located and put the testing on hold. It is possible this round of testing will still take place by the end of the internship if the grips can be found. Overall, this portion of the internship has helped me become familiar with one kind of permeability test as well as a popular tensile/compression testing machine. Finally, I also had the chance to be trained using a metal lathe for making very small tips for a soldering iron. These tips will be used to melt threaded brass inserts into 3D printed plastic. Working with James Brown, I was able to successfully machine a brass rod down to as little as 0.064 inches plus or minus 0.001 inches. It was very rewarding to learn how to best use the machine and become familiar with a skill that will undoubtedly be used again in the future. I have been told by several professional engineers that learning to use a lathe and mill will be invaluable skills in the field. This knocks 50 percent of that goal off and I look forward to learning the mill at some point in the future. As is apparent with this list of projects, my internship was not focused on a single over-arching goal. Instead, I was able to gain experience in a myriad of very different areas. I feel like my time here was spent bouncing from one project to the next. Though sometimes difficult to switch gears, it was very rewarding to be a part of so much in so little time. My career and education will be positively impacted by what I have learned at JSC. My experience with 3D printing has improved my ability to handle many issues that may come up in the future with multiple different technologies. The design work I took part in, especially creating technical drawings, will help me better present designs to any engineer or shop I will encounter. My testing experience has helped me become familiar with a popular kind of tensile test machine that will likely be similar to the kinds I will encounter in the future. Finally, my experience with fabrication has given me a rare opportunity, as an engineer, to take part in the fabrication of a part. This experience will help me better tailor my future designs for the manufacturing process and has given me an appreciation for detailed/delicate machining work. My experience at JSC has been successful and will continue to assist me for a long time within the engineering field.

Zusack, Steven↗

DOE OSTI2020

Porous Membranes for Moisture Probe Protection (SR18024)

In the presence of contaminants, moisture probes can give false moisture readings and have shorter lifetimes. Absolute humidity probes are composed of porous, hygroscopic metallic oxide thin films (Al 2 O 3 ) coupled to electrodes (e.g. Au and Al). While these materials provide absolute humidity readings at low water levels at a relatively low cost, they are sensitive to the presence of contaminants, especially ammonia, due to its high hygroscopicity and ability to bind to the probe. Without frequent recalibration, especially in the presence of contaminants, the humidity levels are inaccurately reported due to measurement drift that occurs when the pores close, changing the impedance of the probe. The goal of this project was to improve the stability and reliability of these moisture probes by incorporating a molecular sieve into the probe to allow only the water to reach the sensor. Molecular sieves contain pores that allow molecule specific permeation. Two dimensional inorganic nanosheets (e.g. BN, MoO 2 , MoS 2 ) have recently been shown to behave as molecular sieves for water. Compared to zeolites, nanoporous materials have higher flux rates through the pores, leading to faster water permeation. Graphene oxide sheets have also been successfully employed for unimpeded water permeation; however, at lower humidity levels, the structure is unstable and the pores shrink, preventing the sieving of molecules. Compared to graphene oxide, sheets based off of inorganic materials, such as molybdenum, have been found to be more stable at lower humidity levels and have faster permeation rates. By creating a barrier in before the Al 2 O 3 sensor chip to prevent the permeation of contaminants into the probe, the lifetime of the probe will be extended. While the molybdenum sheets are a promising material for this application, their performance against ammonia and tritiated compounds have not yet been evaluated. This technology can be applied to other applications, including gas and liquid purification for environmental remediation, single molecule sensors, field effect transistors, and catalysts.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2021

A Novel Technique for Distributed Measuring of Strain in the Vadose Zone

Characterizing water content and pressure changes in the vadose zone is important to understanding a variety of geologic processes, ranging from permeability, to evapotranspiration, and aquifer recharge. Changes in water content, or pressure, cause strain in the solid porous medium of the vadose zone, and it is possible that measuring those strains could be used a characterization tool. The Coherence-length-gated Microwave Photonics Interferometry (CMPI) technique measures strain at high resolution along many intervals defined by pairs of reflectors distributed along an optical fiber. This technique has recently been developed at Clemson University, and it has the spatial, and temporal resolution to characterize the strains that are expected to occur with hydrologic changes in the vadose zone. However, the technique has never been used to measure strain in porous media, so its capabilities remain uncertain. The objective of this thesis is to evaluate the ability of using CMPI to measure strain changes in the vadose zone. The research approach consists of conducting laboratory tests using a column filled with sand that was subjected to changes in water content and pressure. An optical fiber with CMPI reflectors was deployed in a high surface area ribbon and used to measure strain along the axis of the column. The column was made from 8-inch, Schedule 40 PVC pipe (75 cm tall, 20 cm inner diameter) and filled with medium-grained sand (K = 2.5x10-6 m/s, porosity = 0.28, Coefficient of Uniformity = 2, van Genuchten (n = 4.34 and  = 0.00039 m-1), Young’s Modulus = 18 – 47 MPa). Five pressure and four temperature sensors attached to probes inserted into the wall. The optical fiber includes five reflectors spaced 10 cm apart on the inside and outside of the column along the vertical axis. Strain measurements are made between pairs of reflectors. The reflectors are created in 250-micron-diameter acrylate-coated single mode Corning SMF28e+ optical fiber using a femtosecond laser. The optical fiber was laminated between two pieces of polyester film creating a large surface area to transfer strain from the porous media to the optical fiber. The experiments were conducted by filling the column from the bottom or infiltrating water from the top. The water was allowed to equilibrate to room temperature prior to each test in order to limit thermoelastic strain. Five injection tests with a rate of 250 ml/min and three infiltration tests at varying rates were conducted, and the results show patterns of strain and pressure are generally similar. Hydrologic conditions define three zones based on the pressure magnitude and distribution. 1.) Ambient Zone where the pressure heads are quasi-static and the pressure gradient is roughly unity (head gradient of zero). This is the uppermost zone and is characterized by negative pressures. 2.) Transition Zone where the pressures increase from ambient to zero, are changing relatively rapidly and the pressure gradient is relatively steep (pressure head gradients of 2). The Transition zone is 10 to 15 cm thick. 3.) Positive Pressure Zone where the pressure is positive, the rate of change is slower than in the transition zone and the gradient is flatter (pressure head gradient 1.1 to 1.2). This is the lowest zone in the column. Injection of water causes the pressure to increase and the three zones to move upward. The Transition zone moves at a rate of approximately 0.0002 m/s +/- .00005, according to analyses of pressure profiles. This is the same as the average velocity of the water calculated as volumetric flux/effective porosity =5.4x10-5 m/s/0.28. Strain signals in the range of 10s  were observed with a noise level of generally less than 0.1  (signal to noise ratio of greater than 100) during injection and drainage. The spatial and temporal distributions of strain caused by injection depend on the location of the moving pressure zones. The locations of the different pressure zones were determined from pressure profiles at different times and these data were transferred to strain time series. This showed that strain in the Ambient pressure zone is either unchanged or slightly compressive, whereas strain in Transition zone is tensile and roughly proportional to the pressure change, and strain ranges from tensile to compressive in the Positive Pressure zone. In general, the strain is variable at the top of the Positive Pressure zone, but it appears to be consistently tensile lower in the zone. The spatial distribution of strain causes three distinct stages in the strain times series measured between pairs of CMPI reflectors. The strain is unchanged or slightly compressive during Stage 1, it increases (positive strain is tensile) approximately linearly at a rate of 0.02 to 0.03 μ/s during the Stage 2, and then flattens out in Stage 3. The strain increases again during Stage 4 of the time series. The pressure also changes in stages. It is unchanged during Stage 1 and then increases relatively rapidly at a rate of between 4 and 10 Pa/s during Stage 2 and continues to increase during Stages 3 and 4, but at a rate slightly slower than during Stage 2 (from 2.5 to 3.5 Pa/s). The rates of pressure and strain change are consistent with basic analyses. The rate of pressurization is similar to the calculated velocity of flow in the saturated zone, and this is similar to the measured velocity of the strain increase. The ratio of the pressurization rate and strain rate during Stage 2 (2.5 (Pa/s) /0.03 (μ/s)) is 80 MPa, which is approximately equal to the upper range expected considering the uniaxial compression and the Young’s Modulus of the sand. An interesting effect occurs when the upper surface of the sand becomes saturated. Significant compression (several 10s of ) occurs as the pressure and saturation increase at the upper surface. Compression occurs throughout the column, but the effect is greatest at the top of the column. The rate of compression is fastest slightly before ponding occurs, but it slows markedly and nearly stops when water starts to accumulate at the surface (ponding). This effect reverses when the surface of the sand is drained, resulting in tension throughout the column. The compression caused by this effect can be as large or larger than the tensile strain that accumulated during filling. This effect was unexpected because increasing pressure is normally associated with tensile strain. Nevertheless, this effect was observed consistently in all tests where the pressure changes at the upper surface, including tests where water was injected from below or infiltrated from above. This effect behaves as if the pore pressure at the upper surface of the sand exerts a normal force on the boundary (increasing pore pressure exerts a downward compression on the boundary). The results of these laboratory experiments indicate that CMPI can measure strain caused by fluid pressure changes in the vadose zone with a signal to noise ratio of 100 or more. Injection and drainage cause a strain signal that is complex, but repeatable. The magnitudes of the strain signal are consistent with magnitudes that are expected based on poroelastic calculations using independently measured properties of the sand. These results indicate that the CMPI technique with an optical fiber laminated in a polyester ribbon generates data that represent the strain distribution during hydrologic processes of imbibition and drainage in variably saturated sand. This suggests that distributed strain measurements using CMPI could be a viable approach for evaluating processes in the vadose zone, laying the groundwork for future field implementation.

47 OTHER INSTRUMENTATION↗

NASA NTRS1999

Dynamics of Single Chains of Suspended Ferrofluid Particles

We present an experimental study of the dynamics of isolated chains made of super-paramagnetic particles under the influence of a magnetic field. The motivation of this work is to understand if the chain fluctuations exist and, if it does, how does the fluctuation affect chain aggregation. We find that single chains strongly fluctuate and that the characteristic frequency of their fluctuations is inversely proportional to the magnetic field strength. The higher the field the lower the characteristic frequency of the chain fluctuations. In the high magnetic field limit, chains behave like rigid rods without any internal motions. In this work, we used ferrofluid particles suspended in water. These particles do not have any intrinsic magnetization. Once a magnetic field is applied, a dipole moment is induced in each particle, proportional to the magnetic field. A dipolar magnetic interaction then occurs between particles. If dipole-dipole magnetic energy is higher than the thermal energy, the result is a structure change inside the dipolar fluid. The ratio of these two energies is expressed by a coupling constant lambda as: lambda = (pi(a(exp 3))(chi(exp 2))(mu(sub 0))(H(sub 0))(exp 2))/18kT Where a is the particle radius, mu(sub 0) is the vacuum magnetic permeability, H(sub 0) the applied magnetic field, k the Boltzmann constant and T the absolute temperature. If lambda > 1, magnetic particles form chains along the field direction. The lateral coalescence of several chains may form bigger aggregates especially if the particle volume fraction is high. While many studies and applications deal with the rheological properties and the structural changes of these dipolar fluids, this work focuses on the understanding of the chain dynamics. In order to probe the chain dynamics, we used dynamic light scattering (DLS) in self-beating mode as our experimental technique. The experimental geometry is such that the scattering plane is perpendicular to the magnetic field. Therefore, only motions in this plane are probed. A very dilute sample of a ferrofluid emulsion with a particle volume fraction of 10(exp -5) is used in this experiment. We chose such a low volume fraction to avoid multiple light scattering as well as lateral chain-chain aggregation. DLS measures the dynamic structure factor S(q,t) of the sample (q is the scattering wave vector, t is the time). In the absence of the magnetic field, identical particles of ferrofluid droplets are randomly distributed and S(q,t) reduces to exp(-q(exp 2)2D(sub 0)t). D(sub 0)=(kT/(6(pi)(eta)(a)) is the diffusion coefficient of Brownian particles (where Xi = (6(pi)(eta)(a)) is the Stokes frictional coefficient of a spherical particle in a fluid of viscosity eta). If interactions or polydispersity can not be ignored, an effective diffusion coefficient is introduced. Formally, D(sub eff) is defined as: D(sub eff) = - q(exp -2) partial derivative of (ln(S(q,t)) with respect to time, as t goes to 0. D(sub eff) reduces to D(sub 0) if no interactions and only a few particles size are present. Therefore, we can use DLS to measure particle size. The particle radius was found to be a=0.23 mu m with 7% of polydispersity. In this case, if we vary the scattering angle theta (and so q) we do not have any change in the measured diffusion coefficient: it is q-independent. When a magnetic field is applied, particles aggregate into chains if lambda > 1. We first studied the kinetics of the chain formation when lambda = 406. At a fixed scattering angle, we measured diffusion coefficient D(sub eff) as a function of time. Experimentally, we find that D(sub eff) decreases monotonously with time. Physically, this means that chains are becoming longer and longer. Since we are only sensitive to motions in the scattering plane and since chains have their main axis perpendicular to this plane, the measured diffusion coefficient is the trans-verse diffusion coefficient. We can relate D(sub eff) to the mean number of particles per chain N(t) at a given time and to the diffusion coefficient of an isolated particle D(sub 0) as D(sub eff)=f(N(t))D(sub 0). Since f(N) is known from other recent work, N can be expressed as a function of the time. We found a square root dependency: N(t) proportional to the square root of t. As expected for very low volume fraction, this behavior is characteristic of a diffusion-limited aggregation as suggested by several authors and by our previous work. In this study, we focus on the dependence of the effective diffusion coefficient on the scattering angle and the magnetic field strength. After the magnetic field is applied (lambda = 406) for a long time, typically 6 hours, kinetics of chain formation becomes very slow. Chain size does not vary much over the next hour period. Thus, we can perform different interesting experiments. First, at a fixed magnetic field, we measure the effective diffusion coefficient as a function of the scattering angle (from 5 to 130 deg). Our results show that the measured diffusion coefficient increases linearly with the scattering angle: D(sub eff) proportional to q. If we do the same experiment for different lambda values, D(sub eff) depends on lambda as D(sub eff) proportional to lambda(exp -1/2). We also find for different lambda values that the same asymptotic D(sub eff) value is obtained when q approaches zero. The angle dependency of D(sub eff) suggests that an additional motion exists besides chain drifting. Chain size is constant during experiment, which was verified by measuring the same diffusion coefficient at the beginning and at the end of the angle switching. If chains are rigid, D(sub eff) is independent of q. Therefore, we found that D(sub eff) not only measures the motion of the entire chain but also its internal fluctuations. These internal motions are the fluctuations of the particles in the chain. To understand the q dependency of D(sub eff), let us look at the probing length used. In our study, the characteristic length scale probed is l=2pi/q which is in the range of 0.9<l/a<20. When l is much larger than the particle radius (l/a going to infinity) we are mainly sensitive to the center of mass diffusion of the chain. D(sub eff) is then the diffusion of the entire chain and depends only on N but not on q and lambda. The value D(sub eff) allows us to obtain the number of particles per chain N. In the opposite limit (i.e. l/a < 1), we are sensitive to motions on the size of individual particles. The main contributions to the measured diffusion coefficient come from internal motions of the chains (i.e. particles' fluctuations inside the chain). We investigated also the effect of the chain size on D(sub eff). For the same value of the magnetic interaction lambda and different chain sizes, we found that the slope of D(sub eff) versus q decreases when N increases as a power law D(sub eff) proportional to N(exp -0.7). This is an important behavior because this means that the longer the chain the slower its internal fluctuations besides the whole chain motion.

Cutillas, S.↗

DOE OSTI2019

Low cost modular plasma system for reforming of natural gas

The initial aim of this project was to develop a low-cost compact, modularly scalable, point of use, on demand production system for the reforming of natural gas (NG) into products such as acetylene, hydrogen and other related hydrocarbons. Based on a pulsed dielectric barrier discharge (DBD), the fast rising voltage pulses produced by the system causes the dielectric breakdown of the gas to lag behind the rapid voltage increase so that a voltage greater than the static breakdown voltage of the gas, called an overvoltage, is briefly attained. The century long commercial use of the DBD discharge to push the highly endothermic oxygen to ozone reaction served as an additional motivation. The project meets the recommendations of the National Research Council 2007 report on plasma science for a greater investment in low temperature plasma science and engineering. An important finding is that the method investigated has a high specific energy requirement (SER) of the order of 1,000 to 5,000 kWh per kg of hydrogen, and a corresponding low efficiency of only ~0.1 to 0.5% of converting electrical into chemical (ΔH, ΔG) energy. This compares unfavorably with 52 kWh/kgH 2 required for NG thermal plasma reforming, or a pulsed spark discharge, Lotfalipour et. al, and Gao et. al. (For comparison electrolysis of water into hydrogen and oxygen gas requires only 45 to 80kWh/kgH 2 ). This project garnered data with different reactor configurations, materials, gases and mixtures including NG, methane, hydrogen, propane, argon, nitrogen and air, gap sizes ranging from 0.5 to 4.1 mm, electrode areas from 5 to 460 cm, voltages to 27 kV, pulse frequencies to 20 kHz and peak currents into the hundreds of amperes, temperatures to 625 °C and pressures from 15 mbar to 2 bar. An SRS 300 residual gas analyzer (RGA) yielded quadrupole mass spectrometry (QMS) data on the reformate. To analyze the data we extended the public domain software OpenChrom®, Wenig, to QMS data, yielding accurate identification and quantitative data on reformate products. This extension of OpenChrom® is applicable beyond this project and is a significant contribution to the general community of researchers. The documentation is available on the internet, see Whitlock, and a copy has been appended to this report. The main product of methane and natural gas plasma reforming is hydrogen, constituting ~90% of the products, followed by 1% to 10% ethane, propane, ethylene, acetylene and isobutene. Neopentane, propene, butane and pentane constitute less than 1 % of product. Adding a nickel catalyst increases the selectivity for hydrogen. Carbon nanosheets (graphene), a product of commercial interest, were synthesized by plasma reforming of acetylene at low pressure. The reformate analysis shows hat saturated and branched hydrocarbons are favored compared with unsaturated and linear hydrocarbons. For example, ethane, propane, iso-butane, 2-methyl butane, and 2-methyl pentane are produced in higher amounts compared with unsaturated and linear components. At low pressure acetylene and ethylene production rate is higher and propane production lower. We developed a recirculating system in which hydrogen is removed through a permeable membrane as fast as it is being produced by the reactor and the remaining products are recirculated at a high flow rate of several liters per minute. This keeps the concentration of H 2 in the reactor low, while achieving a total output concentration of 79%, high enough for pressure swing adsorption to be used for further purification. The recirculating system could be used with other gas reforming technologies. We report on four different reactors,1) a spark discharge reactor, 2) a standard DBD cylindrical reactor, 3) a small DBD reactor where catalyst powder can be quickly loaded onto a carrier to investigate the effect of the plasma on the catalyst and the effectiveness of the of the catalyst in promoting gas reformation and 4) a configurable DBD reactor to study the performance effects of dielectric selection, electrode gap distance, and electrode/dielectric interface on plasma reactor operation. This project achieved a commercializable 1kW plasma system including reactors a plasma pulse generator and a gas supply module.

03 NATURAL GAS↗

DOE OSTI2025

Williston Basin Resource Study for Commercial-Scale Subsurface Hydrogen Storage

The Energy & Environmental Research Center (EERC), in partnership with the U.S. Department of Energy (DOE) National Energy Technology Laboratory (NETL), the EERC’s State Energy Research Center (SERC), MPLX Operations LLC, and TC Energy Development Holdings Inc. (a subsidiary of TC Energy Corporation), studied the potential for subsurface hydrogen storage and recovery in the Williston Basin of western North Dakota. The project’s goal was to evaluate the feasibility of large-scale, secure geologic H 2 storage to support future hydrogen generation, storage, and use. This work included laboratory testing, H 2 –rock–fluid exposure experiments, literature reviews on H 2 embrittlement, and reservoir modeling and simulations. The study included an assessment of storage potential across three types of storage reservoirs using both reservoir simulation and DOE’s web-based tool SHASTA-HELP (Subsurface Hydrogen Assessment, Storage, and Technology Acceleration – Hydrogen Estimator for Logistical Planning), as well as investigation of potential H 2 production and markets for commercial-scale deployment. Building on prior EERC gas storage research, three storage options were selected for detailed evaluation: the Broom Creek Formation (a clastic saline reservoir), the Dickinson Lodgepole Mounds (DLM) complex (carbonate mud mound structures) of the Lodgepole Formation (an active oil and gas producing reservoir), and the Dunham Salt Interval of the Piper Formation (to be used for engineered salt cavern development). These targets were prioritized based on prior EERC research using datasets related to seal capacity, reservoir quality, mechanical integrity, and injectivity. Exposure tests on Broom Creek and DLM samples showed mineral dissolution and precipitation that increased brine salinity and altered reservoir rock surfaces. Although these results provide useful insight, they are limited by small sample sizes and short-term (30-day) exposure, requiring further study to assess long-term storage integrity. Salt formations were not tested because of their known nonreactivity and established mechanical stability. Results of reservoir simulations performed for a single site demonstrated that the Broom Creek Formation may be capable of receiving up to 42,000 tonnes of injected H 2 over 7 months via one well. H 2 recovery took place over 5 months, resulting in approximately 26,000 tonnes (~62% without cushion gas [CG]). This work suggests water production may be important and subsequent cycles of injection and production may perform more efficiently; however, significant site-specific work in the future is needed to assess actual reservoir performance of injection and withdrawal of H 2 storage. For oil reservoir potential, a multiple-well model was used to simulate injection of approximately 32,000 tonnes of H 2 into a single wellbore while simultaneously producing in place reservoir fluids from four offset wells to maintain reservoir pressure. The simulation results suggested a high recovery (~98%); in addition, cost advantages through existing infrastructure could be realized. Challenges in this reservoir include vi managing gas purity and leakage risks. In both scenarios, production of H 2 takes place in a single-well scenario with 10 cycles (7 months of injection and 5 months of production) over 10 years. Finally, the use of engineered caverns in the Dunhan Salt was evaluated, and the results suggest that while they have a smaller capacity (<1000 tonnes per cavern), they exhibit nearly complete gas recovery (>99%), fast response times, and low purity risk. While caverns in North Dakota may be smaller in capacity, fields can be developed in galleries to accommodate the volumetric needs and rapid turnaround times necessary to meet market demands. Geographic limitations and thin salt intervals in North Dakota may represent less total storage potential than salt domes elsewhere, but significant opportunities exist to expand this market for gas storage in North Dakota. A basinwide assessment was performed to estimate a first-of-its-kind value for H 2 storage on a large scale. DOE’s SHASTA-HELP, combined with EERC simulation work, was used to perform the assessment. Estimated H 2 storage potential varied widely for each formation type. The Broom Creek saline formation was estimated to have a storage potential of approximately 1.7–90.5 million tonnes (MMt). The DLM oil reservoirs were estimated to have 0.07–0.19 MMt of capacity. Notably, each of these estimates relies on significant assumptions regarding reservoir thickness, porosity, permeability, and CG needed for operation. Much research is needed to understand the true site-specific storage resource potential of each formation. Using the Dunham Salt Interval for cavern development may result in as much as 4.79 MMt (up to 2.87 MMt working gas) of H 2 storage potential. An important note for consideration is that the values presented here need significantly more geological characterization and engineering assessments prior to gaining confidence in performance. This will be a focal point for future research and development needs. The basinwide evaluation also indicated that North Dakota has significant H 2 generation potential, with estimates up to a possible 13 MMt annually, suggesting a substantial opportunity for H 2 market development and thus the need for commercial-scale H 2 storage to facilitate growth and resilience. Key Recommendations 1. Conduct detailed site characterization (3D seismic, well logs, core sampling) to reduce geologic uncertainty. 2. Perform techno-economic analyses incorporating market, regulatory, and incentive frameworks. 3. Investigate long-term interactions among H 2 , CGs, well materials, and formations to assess risks. 4. Develop pilot- and field-scale demonstrations to validate models and establish best practices.

03 NATURAL GAS↗

DOE OSTI2019

Initial Assessment of Cover Degradation Features at the Mexican Hat, Utah, UMTRCA Disposal Site - 19556

The Mexican Hat, Utah, Uranium Mill Tailings Radiation Control Act (UMTRCA) Title I Disposal Site is located on the Navajo Reservation in southeast Utah. The US Nuclear Regulatory Commission licensed the site to the US Department of Energy Office of Legacy Management (LM) for custody and long-term care. LM manages long-term surveillance and maintenance activities at the site with the principal goal of protecting human health and the environment. The disposal cell was designed to encapsulate low-level radioactive mill tailings and other residual radioactive materials (RRM) in a way that minimizes the need for active maintenance and limits radon gas emanation and precipitation infiltration. The disposal cell has a multicomponent cover, consisting of a 60 cm thick (24 inch), low-permeability, bentonite-amended radon barrier, overlain by a 15 cm thick (6 inch) sandy gravel bedding/filter layer and a 30 cm thick (12 inch) riprap erosion-protection layer. Under UMTRCA, designs intended to control and contain RRM shall be effective for up to 1000 years, to the extent reasonably achievable and, in any case, for at least 200 years. In 2016, multiple subtle depressions were identified on the rock cover along the toe and lower portions of the northeast side slope of the disposal cell. Due to concerns regarding potential impacts to disposal cell performance and erosion resistance, evaluations of the depressions and cell cover design and construction were initiated. The evaluations included reviews of the disposal cell as-built drawings and supporting design calculations for the rock cover components. Also, in 2017, a weather monitoring station was installed at the site to collect continuous site-specific meteorological data, and repeatable ground-based light imaging, detection, and ranging (lidar) topographical and aerial photogrammetry surveys were implemented to monitor for potential changes in the surface depression features. The evaluations also included visual inspections of the depressions, and in 2018, small-area manual excavations of the rock cover components (test pits) were performed to observe the conditions of the cover components, scan for radioactivity, and observe evidence of erosion on the surface of the radon barrier material. Voids and incisions were discovered within the radon barrier on the north and northeast side slopes of the disposal cell. Visual observations at test pits indicate that the bedding/filter material is highly segregated and may not be in conformance with the disposal cell engineering and construction design specifications. Post-construction development of a weak to strongly cemented material has also been observed immediately below the base of the bedding layer in test pits with observed radon barrier degradation. A series of radiological surveys have been performed at the site, and radiological readings have not exceeded natural background conditions in the vicinity of the site. Thus, the site remains protective of human health and the environment. Implementation of continuous radiological monitoring at the site will be initiated in fall 2018 through the deployment of radon cups and thermoluminescent dosimeters to obtain data that provides supporting evidence that the disposal cell remains protective of human health and the environment. Evaluations to determine the cause(s) of the depression features and associated radon barrier erosion are ongoing. Possible mechanisms of cover degradation identified thus far include segregated bedding material that would allow for higher precipitation runoff velocities, resulting in erosion of the radon barrier; post-construction cementation of radon barrier or aeolian material that could negatively affect the performance of the radon barrier; cation exchange leading to the development of cementation; and aeolian deposition affecting precipitation runoff. Moreover, geotechnical sampling and testing is planned to verify spatial cover conditions relative to design specifications. The resulting information will be used to identify possible causes for the surface depressions and associated radon barrier degradation, gain insight on potential long-term performance implications along the side slopes of the disposal cell, and identify potential corrective actions. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2020

North Dakota Integrated Carbon Storage Complex Feasibility Study. Final report

In spring 2017, the Energy & Environmental Research Center (EERC) initiated an effort to determine the feasibility of developing a commercial-scale CO 2 geologic storage complex able to store 50+ million tonnes (Mt) of CO 2 in central North Dakota safely, permanently, and economically. The objective was to fulfill the goals of the U.S. Department of Energy (DOE) Carbon Storage Assurance Facility Enterprise (CarbonSAFE) Initiative and address technical and nontechnical challenges specific to commercial-scale deployment of a CO2 storage project. The findings clearly show that the concept of capturing CO 2 from a lignite-fired electrical generation facility in central North Dakota and safely and permanently storing the CO 2 in the deep subsurface is indeed technically, economically, and socially feasible. This project evaluated two study areas and their respective geologic storage complexes located adjacent to separate coal-fired facilities in North Dakota: the Basin Electric Power Cooperative (BEPC)-owned Great Plains Synfuels Plant (GPSP) and the Minnkota Power Cooperative (Minnkota)-owned Milton R. Young Station (MRYS). These locations, one with CO 2 capture in place and an existing CO 2 pipeline, are bolstered by progressive North Dakota pore space ownership and long-term liability laws. These elements and a motivated team created an ideal synergistic scenario for ensuring success of the CarbonSAFE Initiative and promoting North Dakota’s statewide vision for carbon management. The project included drilling two new geologic characterization wells, integrating an existing 3-D seismic survey, creating a geologic model subsequently used for injection simulation, a risk assessment, public outreach, and generating a site development plan based on results. In addition, the performance of select National Risk Assessment Partnership tools was evaluated. The geologic characterization wells were drilled ~5600 feet deep to the Broom Creek Formation; ~350 feet of core was retrieved from each well. The core included the Broom Creek (targeted injection zone) and a portion of the overlying Opeche Shale (seal). The Flemmer-1 well, west of Beulah, North Dakota, yielded 169 feet of sandstone. The BNI-1 well located south of Center, North Dakota, yielded 124 feet of sandstone. In each case, laboratory analysis of the sandstone showed permeability in the 300–1000-mD range, with porosity of 20%–30%. The Flemmer-1 well was sited within the boundaries of an existing 3-D seismic survey. Colocating the well with the seismic survey maximized the relationship between new and legacy data and developed a first-of-its-kind interpretation of the geologic fabric of the Broom Creek. Geologic characterization data were integrated into a 5544-mi 2 geocellular model that encompassed both new wells and stratigraphy from the surface to the Amsden Formation (underlying the Broom Creek). The model was later expanded vertically to include the deeper Black Island–Deadwood interval to examine its potential viability as a storage target. The geocellular model provided the foundation for dynamic simulation of CO 2 into the Broom Creek. Results of the simulation suggest that the Broom Creek could accept the DOE target rate of 2 Mt/yr of CO 2 into as few as two wells. To bracket the expected capture from MRYS, simulations were also investigated for a 4-Mt/yr rate near MRYS. Although more wells are needed (two additional), the Broom Creek still has the storage resource to accept the CO 2 at the increased rate. A risk assessment exercise was conducted to identify and assess technical and nontechnical risks that could prevent potential candidate storage complexes within the study area from serving as commercial storage sites. The assessment identified and evaluated six technical risk categories: 1) CO 2 injectivity, 2) storage capacity, 3) lateral migration of CO 2 , 4) lateral pressure propagation, 5) vertical migration of CO 2 or formation brine, and 6) induced seismicity. Following two rounds of analysis and scoring, no risks were determined to preclude continued efforts to develop carbon capture, utilization, and storage (CCUS) in central North Dakota. The risk assessment results will be used to guide future site characterization, modeling and simulation, and monitoring activities. A specific nontechnical strategic risk based on challenges that may be realized in amalgamation of pore space resulted in vertically expanding the geologic model to incorporate the potential for stacked storage in multiple saline reservoirs. By including the Black Island–Deadwood interval (the basal sedimentary reservoir in this region), the amalgamated areal extent could be reduced by as much as 45%. Working with a smaller geographic area reduces risks and costs associated with monitoring and pore space leasing. An economic evaluation incorporating capture; transport (<5 mi); Class VI wells; permitting; and monitoring, verification, and accounting suggests implementing commercial-scale CCUS is economically attractive if the federal tax benefits of 45Q are included. This is validated by Minnkota’s continued pursuit of CO 2 capture and geologic storage at MRYS through its Project Tundra initiative, indicating that there is a business case for CCUS in central North Dakota. Currently, North Dakota is the only state with underground injection control (UIC) Class VI primacy. Built into the North Dakota Century Code is a series of regulatory requirements that guide the process to obtain a Class VI CO 2 storage facility permit. As part of this project, a site development plan was compiled to assure compliance with North Dakota’s requirements to permit a commercial-scale CO 2 storage operation and includes a prospective time line encompassing a general breakdown of activities. In total, an estimated 30 months would be needed to execute the necessary steps to attain a North Dakota CO 2 storage facility permit. Outreach was an integral part of the project and encompassed any project-related activity that had contact or exposure beyond the project team. The goals of outreach were to foster an environment from which stakeholders could make informed decisions about the project and gauge community receptiveness to a CCUS project. A consistent set of messages and outreach products were developed in conjunction with an outreach advisory board that integrated project partners and team members. To gauge public acceptability of geologically storing CO 2 , 5611 households in the project area were invited to participate in an online survey. The survey results indicate that the public attitude regarding CCUS is neutral to positive, with strong sentiment that CO 2 capture and storage may be an approach to maintain the economic vitality of the region. To achieve project objectives, critical support in the form of financial backing, engineering evaluations, site access, outreach collaboration, operations data, risk assessment/evaluation, and software access was provided by BEPC, the North Dakota Industrial Commission Lignite Research Council, ALLETE Clean Energy, BNI Energy, North American Coal Corporation, Minnkota, Prairie Public Broadcasting, Computer Modelling Group Ltd., and Schlumberger.

29 ENERGY PLANNING, POLICY, AND ECONOMY↗

DOE OSTI2013

In-Situ Testing and Performance Assessment of a Redesigned WIPP Panel Closure - 13192

There are two primary regulatory requirements for Panel Closures at the Waste Isolation Pilot Plant (WIPP), the nation's only deep geologic repository for defense related Transuranic (TRU) and Mixed TRU waste. The Federal requirement is through 40 CFR 191 and 194, promulgated by the U.S. Environmental Protection Agency (EPA). The state requirement is regulated through the authority of the Secretary of the New Mexico Environment Department (NMED) under the New Mexico Hazardous Waste Act (HWA), New Mexico Statutes Annotated (NMSA) 1978, chap. 74-4-1 through 74-4-14, in accordance with the New Mexico Hazardous Waste Management Regulations (HWMR), 20.4.1 New Mexico Annotated Code (NMAC). The state regulations are implemented for the operational period of waste emplacement plus 30 years whereas the federal requirements are implemented from the operational period through 10,000 years. The 10,000 year federal requirement is related to the adequate representation of the panel closures in determining long-term performance of the repository. In Condition 1 of the Final Certification Rulemaking for 40 CFR Part 194, the EPA required a specific design for the panel closure system. The U.S. Department of Energy (DOE) Carlsbad Field Office (CBFO) has requested, through the Planned Change Request (PCR) process, that the EPA modify Condition 1 via its rulemaking process. The DOE has also requested, through the Permit Modification Request (PMR) process, that the NMED modify the approved panel closure system specified in Permit Attachment G1. The WIPP facility is carved out of a bedded salt formation 655 meters below the surface of southeast New Mexico. Condition 1 of the Final Certification Rulemaking specifies that the waste panels be closed using Option D which is a combination of a Salado mass concrete (SMC) monolith and an isolation/explosion block wall. The Option D design was also accepted as the panel closure of choice by the NMED. After twelve years of waste handling operations and a greater understanding of the waste and the behavior of the underground salt formation, the DOE has established a revised panel closure design. This revised design meets both the short-term NMED Permit requirements for the operational period, and also the Federal requirements for long-term repository performance. This new design is simpler, easier to construct and has less of an adverse impact on waste disposal operations than the originally approved Option D design. The Panel Closure Redesign is based on: (1) the results of in-situ constructability testing performed to determine run-of-mine salt reconsolidation parameters and how the characteristics of the bedded salt formation affect these parameters and, (2) the results of air flow analysis of the new design to determine that the limit for the migration of Volatile Organic Compounds (VOCs) will be met at the compliance point. Waste panel closures comprise a repository feature that has been represented in WIPP performance assessment (PA) since the original Compliance Certification Application of 1996. Panel closures are included in WIPP PA models principally because they are a part of the disposal system, not because they play a substantive role in inhibiting the release of radionuclides to the outside environment. The 1998 rulemaking that certified WIPP to receive transuranic waste placed conditions on the panel closure design to be implemented in the repository. The revised panel closure design, termed the Run-of-Mine (ROM) Panel Closure System (ROMPCS), is comprised of 30.48 meters of ROM salt with barriers at each end. The ROM salt is generated from ongoing mining operations at the WIPP and may be compacted and/or moistened as it is emplaced in a panel entry. The barriers consist of bulkheads, similar to those currently used in the panels as room closures. A WIPP performance assessment has been completed that incorporates the ROMPCS design into the representation of the repository, and compares repository performance to that achieved with the approved Option D design. Several key physical processes and rock mechanics principles are incorporated into the performance assessment. First, creep closure of the salt rock surrounding a panel entry results in consolidation of the ROM salt emplaced in the entry. Eventually, the ROM salt comprising the ROMPCS will approach a condition similar to intact salt. As the ROM salt reaches higher fractional densities during consolidation, back stress will be imposed on the surrounding rock mass leading to eventual healing of the disturbed rock zone above and below the panel closure. Healing of the disturbed rock zone above and below the ROMPCS reduces the porosity and permeability in those areas. Analysis of the new design demonstrates that: (1) the WIPP continues to meet regulatory compliance requirements when the ROMPCS design is implemented instead of Option D, and (2) there is no impact on the short-term effectiveness of the panel closure to limit the concentration of VOCs at the WIPP site boundary to a fraction of the health-based exposure limits (HBLs) during the operational period. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗