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At least 163 records · Page 9

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DOE OSTI2024

Application of Partial Least Squares Approaches to Pyroprocessing ER Data

Multivariate approaches show promise for application to process monitoring for safeguards of pyroprocessing. Past MPACT work explored the application of Principal Component Analysis (PCA) to detect off-normal conditions in pyroprocessing electrorefiner (ER) data from in the Hot Fuel Examination Facility (HFEF) at Idaho National Laboratory (INL) known as the Scalable Pyrochemical Recycling testbed (SPyRe) ER. PCA, however, does not consider the output variables. In FY24, multivariate analysis was extended from PCA to Partial Least Squares (PLS) analysis. PLS maximizes the variance between both the input signals and output variables. In the case of this work, PLS was applied in two different manners: Predictive PLS and Discriminant PLS. Predictive PLS maximizes the covariance between the process variables of the ER and the measured U concentration from in-situ voltammetry. Discriminant PLS maximizes the covariance between the process variables and a set of training process “states” such as known off-normal conditions. By projecting into the latent variable space in PLS, the process variables can be regressed onto the outputs and predictions can be made for new data sets. In this work, by applying predictive PLS, a penalized non-linear PLS approach was able to make predictions of concentration based on test and training data and detect when operations were off-normal. However, the predictive PLS does not classify the signals to which off-normal operations are attributable. Discriminant PLS can be used to classify off-normal operations but is inadequate to properly classify specific off-normal classes like power supply faults when the Discriminant PLS model is only specifically trained to detect that off-normal class. When all faults are trained against the observation data, all three operational classes are accurately classified and distinguished. Thus, future application of latent variable techniques should not select any given method, but should use a mixture of PCA, Predictive PLS, and Discriminant PLS.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2024

Non-nuclear Component Signatures for Warhead Dismantlement Confirmation

The verification of warhead dismantlement is expected to be an important component in future arms reduction treaties. Historic approaches developed with future arms control treaty verification in mind often involve intrusive measurements, process monitoring, and/or inspector presence to provide confidence that an authentic warhead has been dismantled. This work explores the possibility of reducing the negative impacts of these invasive approaches while also delivering a method that is more likely to provide non-sensitive data that can be shared with not only other nuclear weapons states but also non-nuclear weapons states partners. This work explores a novel approach for verifying dispositioned non-nuclear weapon components, providing confidence post-dismantlement that a treaty accountable item that was dismantled was in fact a treaty-relevant nuclear weapon system as declared. This method provides an alternative to intrusive inspection processes in nuclear weapons production environments, which would require significant changes to the host’s operational behaviors. It achieves this by identifying intrinsic neutron-induced signatures of non-nuclear components to determine their authenticity and estimate the duration they were exposed within a nuclear weapons system using technologies that are already in use for other national security applications. Intrinsic radiation effects studies are already a part of the stockpile aging and surveillance evaluations. However, none of these technologies and approaches have been previously considered for verification applications of non-nuclear component disposition. In this report, we introduce modeling studies that have been used to identify the most promising candidate parts and materials with signatures that are measurable and actionable. These models have been validated with laboratory measurements of signatures induced by the exposure of candidate materials to neutrons over a range of times. Predictive modeling then demonstrates the methodology for estimating exposure times and/or limits. Laboratory measurements of authentic non-nuclear parts from a dismantled warhead demonstrate the feasibility of employing these signature measurements. And finally, a concept of operations (CONOPS) for the potential use of this methodology is presented.

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗

NASA NTRS1994

A Distance Measure for Attention Focusing and Anomaly Detection in Systems Monitoring

Any attempt to introduce automation into the monitoring of complex physical systems must start from a robust anomaly detection capability. This task is far from straightforward, for a single definition of what constitutes an anomaly is difficult to come by. In addition, to make the monitoring process efficient, and to avoid the potential for information overload on human operators, attention focusing must also be addressed. When an anomaly occurs, more often than not several sensors are affected, and the partially redundant information they provide can be confusing, particularly in a crisis situation where a response is needed quickly. Previous results on extending traditional anomaly detection techniques are summarized. The focus of this paper is a new technique for attention focusing.

attention focusing systems monitoring anomaly dete↗

DOE OSTI2024

Portable fiber optic sensor for rare earth elements and other critical metals using photoluminescence methods

Rare earth elements and other metals are vital to a range of technologies that are used in the energy and defense sectors. However, monopolistic market conditions have caused significant concern over the stability of the critical metal supply chain, and this has spurred extensive efforts in many nations to produce these metals domestically, both from conventional sources such as mining and well as from unconventional sources such as coal and its utilization byproducts. Slow and expensive characterization methods pose a significant barrier for both metals prospecting and process monitoring. A promising solution to this challenge is the development of highly sensitive luminescent sensors for metals, which can offer low costs, portability, and sensitivity. Anionic zinc adeninate metal-organic frameworks (BioMOFs) are known to distinguishing and detect part-per-billion levels of terbium, europium, samarium, and dysprosium in water by sensitizing the narrow, element-specific emission bands from these lanthanides. Here, a BioMOF material is immobilized onto a large diameter, solarization-resistant fiber optic tip integrated with a portable, low-cost spectrometer for rare earth element sensing. Immobilizing the sensing material on fiber instead of dispersing the sensing material in solution offers several advantages: it facilitates solvent removal, which enhances luminescent signal from the sensitized lanthanides, and it also allows the BioMOF to be recycled for multiple uses. The sensing system was deployed on a simulated process stream and exhibited qualitative agreement with inductively-coupled plasma mass spectrometry for terbium and europium detection, highlighting the potential for the sensing system to be deployed for real-world applications. By using different sensing materials, the same portable sensor may be deployed to detect other energy relevant metals such as cobalt, providing a cost-effective and sensitive platform for critical metal characterization.

Crawford, Scott↗

NASA NTRS2005

Encryption for Remote Control via Internet or Intranet

A data-communication protocol has been devised to enable secure, reliable remote control of processes and equipment via a collision-based network, while using minimal bandwidth and computation. The network could be the Internet or an intranet. Control is made secure by use of both a password and a dynamic key, which is sent transparently to a remote user by the controlled computer (that is, the computer, located at the site of the equipment or process to be controlled, that exerts direct control over the process). The protocol functions in the presence of network latency, overcomes errors caused by missed dynamic keys, and defeats attempts by unauthorized remote users to gain control. The protocol is not suitable for real-time control, but is well suited for applications in which control latencies up to about 0.5 second are acceptable. The encryption scheme involves the use of both a dynamic and a private key, without any additional overhead that would degrade performance. The dynamic key is embedded in the equipment- or process-monitor data packets sent out by the controlled computer: in other words, the dynamic key is a subset of the data in each such data packet. The controlled computer maintains a history of the last 3 to 5 data packets for use in decrypting incoming control commands. In addition, the controlled computer records a private key (password) that is given to the remote computer. The encrypted incoming command is permuted by both the dynamic and private key. A person who records the command data in a given packet for hostile purposes cannot use that packet after the public key expires (typically within 3 seconds). Even a person in possession of an unauthorized copy of the command/remote-display software cannot use that software in the absence of the password. The use of a dynamic key embedded in the outgoing data makes the central-processing unit overhead very small. The use of a National Instruments DataSocket(TradeMark) (or equivalent) protocol or the User Datagram Protocol makes it possible to obtain reasonably short response times: Typical response times in event-driven control, using packets sized .300 bytes, are <0.2 second for commands issued from locations anywhere on Earth. The protocol requires that control commands represent absolute values of controlled parameters (e.g., a specified temperature), as distinguished from changes in values of controlled parameters (e.g., a specified increment of temperature). Each command is issued three or more times to ensure delivery in crowded networks. The use of absolute-value commands prevents additional (redundant) commands from causing trouble. Because a remote controlling computer receives "talkback" in the form of data packets from the controlled computer, typically within a time interval < or =1 s, the controlling computer can re-issue a command if network failure has occurred. The controlled computer, the process or equipment that it controls, and any human operator(s) at the site of the controlled equipment or process should be equipped with safety measures to prevent damage to equipment or injury to humans. These features could be a combination of software, external hardware, and intervention by the human operator(s). The protocol is not fail-safe, but by adopting these safety measures as part of the protocol, one makes the protocol a robust means of controlling remote processes and equipment by use of typical office computers via intranets and/or the Internet.

Lineberger, Lewis↗

NASA NTRS2010

Electrochemical Detection of Multiple Bioprocess Analytes

An apparatus that includes highly miniaturized thin-film electrochemical sensor array has been demonstrated as a prototype of instruments for simultaneous detection of multiple substances of interest (analytes) and measurement of acidity or alkalinity in bioprocess streams. Measurements of pH and of concentrations of nutrients and wastes in cell-culture media, made by use of these instruments, are to be used as feedback for optimizing the growth of cells or the production of desired substances by the cultured cells. The apparatus is designed to utilize samples of minimal volume so as to minimize any perturbation of monitored processes. The apparatus can function in a potentiometric mode (for measuring pH), an amperometric mode (detecting analytes via oxidation/reduction reactions), or both. The sensor array is planar and includes multiple thin-film microelectrodes covered with hydrous iridium oxide. The oxide layer on each electrode serves as both a protective and electrochemical transducing layer. In its transducing role, the oxide provides electrical conductivity for amperometric measurement or pH response for potentiometric measurement. The oxide on an electrode can also serve as a matrix for one or more enzymes that render the electrode sensitive to a specific analyte. In addition to transducing electrodes, the array includes electrodes for potential control. The array can be fabricated by techniques familiar to the microelectronics industry. The sensor array is housed in a thin-film liquid-flow cell that has a total volume of about 100 mL. The flow cell is connected to a computer-controlled subsystem that periodically draws samples from the bioprocess stream to be monitored. Before entering the cell, each 100-mL sample is subjected to tangential-flow filtration to remove particles. In the present version of the apparatus, the electrodes are operated under control by a potentiostat and are used to simultaneously measure the pH and the concentration of glucose. It is anticipated that development of procedures for trapping more enzymes into hydrous iridium oxide (and possibly into other electroactive metal oxides) and of means for imparting long-term stability to the transducer layers should make it possible to monitor concentrations of products of many enzyme reactions for example, such key bioprocess analytes as amino acids, vitamins, lactose, and acetate.

Rauh, R. David↗

DOE OSTI2025

Monitoring Sulfuric Acid and Temperature Using Raman Spectroscopy and Multivariate Chemometrics

Multivariate regression models were optimized for the quantification of sulfuric acid (H 2 SO 4 ) [0–8 M] and temperature (20 °C–80 °C) in the presence of ammonium sulfate ((NH 4 ) 2 SO 4 [0–0.6 M]) using Raman spectroscopy. Optical vibrational spectroscopy is a useful nondestructive technique for the in situ analysis of complex chemical systems notoriously difficult to monitor in situ and in real-time. Multivariate analysis, a chemometrics method, can be paired with these nondestructive optical methods for determining analyte concentration and speciation in complex solutions, such as dissociated species in polyprotic acids, e.g., H 2 SO 4 . The effect of temperature is often overlooked although it can have a major influence on speciation and the corresponding Raman spectra. Here, in this study, partial least squares regression models were optimized for the quantification of H 2 SO 4 and its two deprotonated forms as a function of temperature. Measuring bisulfate as a function of temperature is particularly challenging owing to changes in the second dissociation constant. A designed training set effectively minimized the sample set size and trained a robust predictive model with percent root mean square error of <3% for H 2 SO 4 . The practical strategy employed here was demonstrated to be effective for building chemometric models that directly account for dynamic temperatures with static samples and is shown to be amenable to flow cell analysis applications with a simple calibration transfer for process monitoring applications.

D-optimal design↗

DOE OSTI2024

Automated Calibration for Rapid Optical Spectroscopy Sensor Development for Online Monitoring

An automated platform has been developed to assist researchers in the rapid development of optical spectroscopy sensors to quantify species from spectral data. This platform performs calibration and validation measurements simultaneously. Real-time, in situ monitoring of complex systems through optical spectroscopy has been shown to be a useful tool; however, building calibration models requires development time, which can be a limiting factor in the case of radiological or otherwise hazardous systems. While calibration time can be reduced through optimized design of experiments, this study approached the challenge differently through automation. The ATLAS (Automated Transient Learning for Applied Sensors) platform used pneumatic control of stock solutions to cycle flow profiles through desired calibration concentrations for multivariate model construction. Additionally, the transients between desired concentrations based on flow calculations were used as validation measurements to understand model predictive capabilities. This automated approach yielded an incredible 76% reduction in model development time and a 60% reduction in sample volume versus estimated manual sample preparation and static measurements. The ATLAS system was demonstrated on two systems: a three-lanthanide system with Pr/Nd/Ho representing a use case with significant overlap or interference between analyte signatures and an alternate system containing Pr/Nd/Ni to demonstrate a use case in which broad-band corrosion species signatures interfered with more distinct lanthanide absorbance profiles. Both systems resulted in strong model prediction performance (RMSEP < 9%). Lastly, ATLAS was demonstrated as a tool to simulate process monitoring scenarios (e.g., column separation) in which models can be further optimized to account for day-to-day changes as necessary (e.g., baseline correction). Ultimately, ATLAS offers a vital tool to rapidly screen monitoring methods, investigate sensor fusion, and explore more complex systems (i.e., larger numbers of species).

47 OTHER INSTRUMENTATION↗

DOE OSTI2025

Lithium isotopic analysis in depleted lithium salts

Lithium isotope separation processes require characterization of the isotopic compositions of the different output phases of the process. While considerable effort to develop isotope separation methods has been ongoing for decades, the analytical methods associated with these analyses are rarely provided. Here, in this work three types of mass spectrometers (Q-ICP-MS, MC-ICP-MS, TIMS) were tested for the ability to measure depleted lithium salts that are relevant materials for isotopic separations. Results indicate that, once stabilized, the Q-ICP-MS can provide equal precision for Li isotopic samples compared to TIMS or MC-ICP-MS. However, MC-ICP-MS consistently provides the highest precision for salts across both depleted and natural isotopic abundances. These data demonstrate that Q-ICP-MS is an appropriate choice for analysis of depleted lithium salts, especially when rapid analyses are desired for online process monitoring.

07 ISOTOPE AND RADIATION SOURCES↗

DOE OSTI2025

New Era Towards Autonomous Additive Manufacturing: A Review of Recent Trends and Future Perspectives

Abstract The Additive Manufacturing (AM) landscape has significantly transformed in alignment with Industry 4.0 principles, primarily driven by the integration of Artificial Intelligence (AI) and Digital Twin (DT). However, current Intelligent Additive Manufacturing (IAM) systems face limitations such as fragmented AI tool usage and suboptimal human-machine interaction (HMI). This paper reviews existing IAM solutions, emphasizing control, monitoring, process autonomy, and end-to-end integration, and identifies key limitations, such as the absence of a high-level controller for global decision-making. To address these gaps, we propose a transition from IAM to Autonomous Additive Manufacturing (AAM), featuring a hierarchical framework with four integrated layers: knowledge, generative solution, operational, and cognitive. In the cognitive layer, AI agents notably enable machines to independently observe, analyze, plan, and execute operations that traditionally require human intervention. These capabilities streamline production processes and expand the possibilities for innovation, particularly in sectors like in-space manufacturing (ISM). Additionally, this paper discusses the role of AI in self-optimization and lifelong learning, positing that the future of AM will be characterized by a symbiotic relationship between human expertise and advanced autonomy, fostering a more adaptive, resilient manufacturing ecosystem.

Fan, Haolin↗

DOE OSTI2025

A split ribozyme system for in vivo plant RNA imaging and genetic engineering

RNA plays a central role in plants, governing various cellular and physiological processes. Monitoring its dynamic abundance provides a discerning understanding of molecular mechanisms underlying plant responses to internal (developmental) and external (environmental) stimuli, paving the way for advances in plant biotechnology to engineer crops with improved resilience, quality and productivity. In general, traditional methods for analysis of RNA abundance in plants require destructive, labour-intensive and time-consuming assays. To overcome these limitations, we developed a transformative innovation for in vivo RNA imaging in plants. Specifically, we established a synthetic split ribozyme system that converts various RNA signals to orthogonal protein outputs, enabling in vivo visualisation of various RNA signals in plants. We demonstrated the utility of this system in transient expression experiments (i.e., leaf infiltration in Nicotiana benthamiana ) to detect RNAs derived from transgenes and tobacco rattle virus, respectively. Also, we successfully engineered a split ribozyme-based biosensor in Arabidopsis thaliana for in vivo visualisation of endogenous gene expression at the cellular level, demonstrating the feasibility of multi-scale (e.g., cellular and tissue level) RNA imaging in plants. Furthermore, we developed a platform for easy incorporation of different protein outputs, allowing for flexible choice of reporters to optimise the detection of target RNAs.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2025

Real-time single-element-detection structured illumination optical metrology for laser powder bed fusion

Laser powder bed fusion (LPBF) is a type of metal additive manufacturing which could benefit from improved process monitoring to improve quality control. We demonstrate, for the first time to our knowledge, the coaxial monitoring of melt track formation in steel powder with spatial frequency modulation imaging (SPIFI), an enhanced-resolution imaging technique which uses a photodiode to record one-dimensional images. Using a custom live-display software and a high-speed SPIFI geometry, we offset the SPIFI field of view from the fusing beam to monitor different regions of the LPBF melt pool and surrounding area. This demonstrates the potential of SPIFI to monitor spatial features within the melt pool in real-time with increased data efficiency.

Hunter, Scott (ORCID:0009000886150312)↗

DOE OSTI2025

Chloride-Based Volatility for Waste Reduction and/or Reuse of Metallic-, Oxide- and Salt-Based Reactor Fuels

The objective of the chloride based volatility project (CBV) was to demonstrate the ability to separate uranium from used fuel to enable process improvements resulting in 10x reduction of waste volume, while maintaining safeguards standards and global backend costs at $\$$1/MW-hr. Current industrial practices perform separations of used fuel using solvent media in the form of aqueous and molten salt processes, resulting in contaminated process waste. The CBV approach utilized solid state chemistry with no solvent media and was successful in chlorinating uranium and fission product oxides that sublimed into the gas phase and were collected in targeted condensation zones based on temperature gradients of chlorinated products. Recovery of better than 95% of initial uranium in the form of UCl4 was demonstrated when simulated used nuclear fuel was used. Laser induced breakdown spectroscopy, LIBS, and ultraviolet-visible spectroscopy, UV-Vis, were combined into a high temperature flow cell design and utilized as process monitoring techniques to observed chlorinated products leave the reaction vessel in real time.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2026

Virtual Inspection of Advanced Manufacturing via Process-Scale Digital Twins (Abbreviated Report)

Inspection and certification comprise the most significant bottlenecks in advanced manufacturing for NNSA applications, often requiring far more time and resources than the fabrication of the parts themselves. Traditional methods, such as manual review and X-ray computed tomography, are not only slow and costly, but also struggle to provide a clear connection between manufacturing instructions and the final performance of critical components. This gap limits both the agility and assurance needed to support the modernization and safety of the United States nuclear stockpile. In response, our Strategic Initiative established a digital twin framework that integrates realtime process monitoring, automated data analysis, and immersive virtual reality collaboration into a unified inspection pipeline. By leveraging data from sensors, machine instructions, and imaging, we created high-fidelity virtual models of manufactured parts that could be rapidly analyzed and certified. This approach was first demonstrated with Direct Ink Write, and then extended to other manufacturing settings, including conventional (or “subtractive”) manufacturing and to predict the end of life performance of parts per the aging and lifetimes programs. The result is a transformational capability: inspection times have been reduced by a factor of 120,000 without loss of accuracy and while simultaneously improving traceability and confidence in part quality. This framework not only streamlines certification for critical applications, but also positions the national security enterprise to respond more flexibly to emerging challenges, supporting agile manufacturing and digital engineering practices across a broad range of mission-relevant domains.

42 ENGINEERING↗

DOE OSTI2026

Enhanced Preparation for Intelligent Cybermanufacturing Systems (EPICS)

Opportunities exist for realizing transformative advances in productivity and reductions in energy footprint through ubiquitous sensing in manufacturing environments. Enhanced Preparation for Intelligent Cybermanufacturing Systems (EPICS) is a 21-month (4 academic semesters, plus one summer) experience for graduate students that focuses on scaling the knowledge, understanding and leadership skills in the cyber manufacturing area. Masters students (8/year, 32 total) complete 2-year projects on industrially-driven project topics, rotating to internships in summer semester to work on scoping and implementation at project partners. Students complete academic training in embedded systems, process modeling, data science, and cloud-based systems design. Their projects are targeted toward sensor retrofit, process monitoring, root cause analysis, and sensor fusion.

Advanced Manufacturing↗

NASA NTRS1977

Instrumentation and data acquisition systems

A comprehensive and integrated measurement system was identified and a design and development effort initiated to meet the criteria imposed by the National Transonic Facility operating environment. Specific measurement areas receiving concentrated attention include: data acquisition, force measurement, pressure instrumentation, flow visualization techniques, model attitude and model deformation measurement, and temperature measurement. The NTF instrument complex will be centered around four 32-bit, 1-microsecond-cycle-time central processing units connected in a multipoint-distributed network configuration. The principal activities to be supported by these computers are: (1) data base management and processing; (2) research measurement data acquisition and display; (3) tunnel and model control; and (4) process monitoring and communication control. The distributed network approach was chosen to modularize the functional software into definable and implementable parts by the various groups involved in the design and to permit use of similar hardware configurations to improve reliability and maintainability.

Guarino, J. F.↗

NASA NTRS1979

Coal mining with a liquid solvent

Study suggests carbonated water can dissolve or suspend coal and carry it to surface. Mixture of carbon dioxide and water may be coal solvent that will make unmanned mining reality. When used with proposed process monitoring coal solubility with conventional strain gage, solvent is basis for rapid cost effective extraction of coal from underground seams.

Lawson, D. D.↗

NASA NTRS1983

Surface and allied studies in silicon solar cells

Two main results are presented. The first deals with a simple method that determines the minority-carrier lifetime and the effective surface recombination velocity of the quasi-neutral base of silicon solar cells. The method requires the observation of only a single transient, and is amenable to automation for in-process monitoring in manufacturing. This method, which is called short-circuit current decay, avoids distortion in the observed transient and consequent inacccuracies that arise from the presence of mobile holes and electrons stored in the p/n junction spacecharge region at the initial instant of the transient. The second main result consists in a formulation of the relevant boundary-value problems that resembles that used in linear two-port network theory. This formulation enables comparisons to be made among various contending methods for measuring material parameters of p/n junction devices, and enables the option of putting the description in the time domain of the transient studies in the form of an infinite series, although closed-form solutions are also possible.

Lindholm, F. A.↗