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DOE OSTI2020

Retrospective on Recent DOE-Funded Studies Concerning the Extraction of Rare Earth Elements & Lithium from Geothermal Brines (Final Report)

Rare earth elements (REE) and lithium are non-toxic metals that are considered critical materials due to their use in electronics, magnets, batteries, and a wide variety of industrial processes important for the economy and military preparedness. Demand for REE and lithium is increasing and these critical materials are imported, so identifying and exploiting domestic sources of REE and lithium is a national priority. The U.S. Department of Energy (DOE) Geothermal Technologies Office (GTO) has been in the forefront of sponsoring research investigating the potential recovery of REE, lithium, and other critical minerals from geothermal brines. It has been proposed that the future of geothermal energy should include “hybrid systems” that combine electricity generation with other revenue-generating activities, such as recovery of valuable and critical minerals, including REE and lithium. Two recent GTO funding opportunities have focused on the recovery of REE and other valuable minerals from geothermal brines. The research supported by the GTO’s mineral recovery program is focused on three areas: resource characterization, technology for the extraction of REE, and technology for the extraction of lithium (Tables 1 and 2). This report is a retrospective study examining the outcome of GTO’s two recent mineral recovery programs (DE-FOA-0001016 in FY 2014 and DE-FOA-0001376 in FY 2016). In this report, the knowledge, technology, and techniques that were developed by researchers funded by GTO are summarized and discussed. Four projects were funded to assess the concentrations and amounts of REE found in geothermal brines and oil field produced waters. The GTO-funded studies compiled publically available data on REE concentrations from brines and produced water from all over the USA. In addition, new samples were collected and characterized from major geothermal and hydrocarbon basins in the Western USA. The studies examined the relationship between lithology and REE concentrations and developed models examining the influence of geology on REE concentrations in produced brines. It was determined that REE are frequently found at higher concentrations in oil field produced water than geothermal brines, but that some geothermal areas had significant REE resources. Significant reservoirs of REE were identified in the Western USA. In some cases, concentrations of REE were more than 1000 times the concentrations found in seawater. Collectively, these studies represent a comprehensive picture of REE resources associated with geothermal and hydrocarbon systems in the USA. The studies did not examine lithium resources, but in some cases, lithium concentration data was collected. Data from these studies are housed in the Geothermal Data Repository (GDR) and represent a significant information resource and it is recommended that these data be further analyzed in a future study. Eight projects were funded to develop new technology for REE extraction from geothermal fluids. These projects investigated sorption as an approach for removal and recovery of REE from geothermal brines. The projects investigated cutting-edge technology for selective sorption of ions from complex solutions, including the application of metal-organic frameworks and biosorbent proteins. The REE sorption studies tested different combinations of metal-binding ligands and solid supports. The most promising metal-binding ligands for REE included phosphonic acid, thiol, and carboxylic acid functional groups. Ligands were attached or incorporated into a wide variety of solid supports. In most cases, attachment was via covalent bonding to organic resins, polymers, or silica-based supports. Most of the REE projects were conducted at a low technology readiness level (TRL) and showed promise, but direct comparison between technologies was not possible based on the available information. It is recommended that testing and reporting be standardized to the extent possible to facilitate comparisons between technologies. Two projects were directed at novel lithium extraction technology. Both projects investigated the use of inorganic sorbents, including manganese oxides. One study also examined the use of metal- ion imprinted polymers as selective ion-exchange resins for the separation of lithium and manganese from brines. Both approaches showed promise for the selective extraction of lithium from brines, including potentially geothermal brines. Results from these GTO studies indicated that selective REE and lithium extraction is possible, but interference from co-occurring solutes, such as calcium, magnesium, or heavy metals, will interfere with process efficiency and negatively impact process economics. Techno-economic analysis conducted as part of the resource and technology studies suggest extraction of REE from geothermal brines is unlikely to be economically viable, especially since non-geothermal produced waters frequently have higher REE concentrations. It is recommended that benchmarks for techno-economic analysis be established to the extent possible for future studies, to facilitate direct comparison of various technologies. Based on the collective results of this program, it appears that hybrid geothermal power would benefit more from recovery of lithium and other metals, rather than REE. It is recommended that future studies be conducted at a higher- TRL and that sorbents be tested against actual geothermal fluid samples. Prior higher-TRL efforts to extract metals from geothermal brines should be further evaluated for lessons learned.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Drying of Spent Nuclear Fuel: Considerations and Examples

A recently revised American Society for Testing and Materials consensus standard guide for drying of spent nuclear fuel (SNF) provides considerations and guidance for preparing SNF for its safe storage in a sealed dry storage system. The standard discusses (1) needs for drying, (2) techniques to dry, and (3) demonstration of adequate dryness. No specific approach is prescribed since the effective techniques and needs for drying depend on the specifics of the fuel and dry storage system. Here, this paper discusses these topics using examples for both Zr-alloy-clad commercial SNF and for aluminum-alloy-clad research reactor SNF. Residual water can include free water (liquid and/or vapor), physisorbed water bound to internal surfaces, and chemisorbed water incorporated into surface films, such as (oxy)hydroxides. The potential impacts of these residual waters are corrosion/oxidation, radiolytic breakdown into gaseous and/or reactive species, and canister pressurization. For commercial SNF, inadvertent free water, even up to large amounts (e.g., 10+ mol), is not predicted to cause adverse corrosion degradation, except possible fuel oxidation for breached SNF. For aluminum-clad SNF, the production of radiolytic hydrogen with contribution from the chemisorbed water in its hydrated oxides is a primary consideration. For both SNF systems, canister pressurization is predicted to be well within the canister design, and flammability would not pose a safety concern using an oxygen limit of 5 vol % criterion. (Flammability control can be achieved by limiting either hydrogen or oxygen, and an oxygen limit is expected to be easier to meet in the presence of radiolytic H 2 generation.) The two primary technologies for SNF drying, vacuum drying and forced-gas dehydration, are described herein, and drying tests and campaigns using these methods are cited. Dryness criteria and the methods used to detect and measure residual (free) water are also discussed.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2023

Survey of the mechanical and physical behaviors of yttria-stabilized zirconia from multiple dental laboratories

Background: When selecting zirconia for a dental restoration, laboratory prescriptions often refer to high strength and high translucency. In this survey, zirconia specimens were ordered from various dental laboratories for posterior (high strength) and anterior (high translucency) clinical indications. The specimens were then tested and evaluated for their mechanical and physical behaviors. Methods: In a double-blinded manner, 9 laboratories provided 32 specimens from 17 different zirconia blanks, which were tested in the American Dental Association laboratory. Flexural strength tests were performed on standard specimens, and fracture surfaces were examined using both optical and scanning electron microscopy. Chemical composition, Vickers hardness, and absolute transmittance measurements were also performed. Results: A large scatter in the strength values was observed. The zirconia intended for posterior applications displayed strengths (SD) from 195 through 783 MPa (490 [183] MPa), which overlapped greatly with the strengths (SD) of the zirconia intended for anterior applications, 320 through 768 MPa (581 [136] MPa). However, when the strength values were recalculated on the basis of yttria content, the strengths (SD) were 584 (158) MPa for 3 mol% yttria and 373 (104) MPa for 5 mol% yttria. Conclusions: When a prescription was given to dental laboratories to request zirconia on the basis of clinical requirements, there was a large scatter and no consistency in the resulting strength values partly because of mixed use of 3 mol% and 5 mol% yttria zirconia. The 3 mol% materials had much higher strength when the strength values were grouped according to yttria content. Strength was also highly dependent on processing and finishing at the dental laboratories.

3 mol% yttria-tetragonal zirconia polycrystal (3Y-↗
DOE OSTI2021

Trace explosives sampling for security applications (TESSA) study: Evaluation of procedures and methodology for contact sampling efficiency

We report the detection of trace amounts of explosive materials is critical to the security at mass transit centers (e.g., airports and railway stations). In a typical screening process, a trap is used to probe a surface of interest to collect and transfer particulate residue to a detector for analysis. The collection of residues from the surface being probed is widely viewed as the limiting step in this process. A multi-institutional study was performed to establish a methodology for the evaluation of sampling media collection efficiencies. Dry deposited residues of 1,3,5-trinitroperhydro-1,3,5-triazine (RDX), C-4 (an RDX-based explosive), and pentaerythritol tetranitrate (PETN) were harvested from acrylonitrile butadiene styrene (ABS) plastic, ballistic nylon (NYL), and uncoated aluminum surfaces using muslin, Texwipe cotton, and stainless-steel mesh traps. Transfer and collection efficiencies of the sample media were calculated based on liquid chromatography-mass spectrometry analysis. Dry transfer efficiencies (DTE%) to all tested surfaces were greater than 75%, with transfer to ABS plastic being the lowest. Collection efficiency (CE%) varied significantly across the traps and the surfaces, yet some conclusions can be drawn; nylon had the lowest CE% for all cases (~10%), and the stainless steel mesh had the lowest CE% for the evaluated traps (~20%). Though the testing parameters have been standardized among the participants to establish a framework for an independent comparison of contact sampling media and surfaces, substantial variations in the DTE% and the CE% were observed, suggesting that other variables can affect contact sampling.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Energy and mobility impacts of connected autonomous vehicles with co-optimization of speed and powertrain on mixed vehicle platoons

Intersections are known to be traffic bottlenecks where a significant amount of energy consumption could be caused due to deceleration/acceleration in the presence of red signals. With an increased level of connectivity and automation of intelligent transportation systems, connected autonomous vehicles (CAVs) are expected to be able to proactively adjust their driving strategies subject to constraints imposed by the predicted future traffic. As a result, many potential benefits can be achieved, such as improved energy efficiency, enhanced traffic safety, among many others. Notably, the way CAVs are controlled affects the following legacy vehicles (LVs) due to complex traffic dynamics. Here, we are particularly interested in studying the energy and mobility impact of CAVs with an improved traffic prediction method on mixed vehicle platoons at various market penetration rates. Leveraging traffic prediction, CAVs are controlled with co-optimization of their speed and gear position. Specifically, a traffic prediction framework in a rolling horizon fashion is employed based upon a modified Payne–Whitham (PW) model capable of handling mixed traffic consisting of CAVs and LVs. The prediction error of the modified PW model is reduced by 53.62% compared to that of the standard PW model under test scenarios. According to the predicted traffic conditions, speed and gear position of CAVs are co-optimized with the primary goal of minimizing energy consumption when driving on a signalized arterial. The energy benefits achieved by CAVs and the impact of CAVs on LVs behind are studied comprehensively for mixed vehicle platoons. The lead LV follows a real-world speed profile collected on TH-55 in Minnesota. Numerical results show that energy benefits achieved by the vehicle platoon range from 2% to 16%, and a 1% to 5% reduction in travel time for LVs behind CAVs is also observed, at different penetration rates of CAVs in various traffic scenarios. Furthermore, it is observed that CAVs using the proposed eco-driving approach appear to have a positive impact on the LVs behind in terms of energy consumption, regardless of the driving styles of the LVs ahead.

33 ADVANCED PROPULSION SYSTEMS↗
DOE OSTI2026

Reconstructing Quasar Spectra and Measuring the Lyα Forest with SpenderQ

Quasar spectra carry the imprint of foreground intergalactic medium (IGM) through absorption features. In particular, absorption caused by neutral hydrogen gas, the "Lyα forest," is a key spectroscopic tracer for cosmological analyses used to measure cosmic expansion and test physics beyond the standard model. Despite their importance, current methods for measuring Lyα absorption cannot directly derive the intrinsic quasar continuum and make strong assumptions on its shape, thus distorting the measured Lyα clustering. We present SpenderQ , a ML-based approach for directly reconstructing the intrinsic quasar spectra and measuring the Lyα forest from observations. SpenderQ uses the Spender spectrum autoencoder to learn a compact and redshift-invariant latent encoding of quasar spectra, combined with an iterative procedure to identify and mask absorption regions. To demonstrate its performance, we apply SpenderQ to 400,000 synthetic quasar spectra created to validate the Dark Energy Spectroscopic Instrument Year 1 Lyα cosmological analyses. SpenderQ accurately reconstructs the true intrinsic quasar spectra, including the broad Lyβ, Lyα, SiIV, CIV, and CIII emission lines. Redward of Lyα, SpenderQ provides percent-level reconstructions of the true quasar spectra. Blueward of Lyα, SpenderQ reconstructs the true spectra to < 5%. SpenderQ reproduces the shapes of individual quasar spectra more robustly than the current state-of-the-art. We, thus, expect it will significantly reduce biases in Lyα clustering measurements and enable studies of quasars and their physical properties. SpenderQ also provides informative latent variable encodings that can be used to, e.g., classify quasars with Broad Absorption Lines. Overall, SpenderQ provides a new data-driven approach for unbiased Lyα forest measurements in cosmological, quasar, and IGM studies.

Hahn, ChangHoon [Arizona U., Astron. Dept. - Stewa↗
DOE OSTI2024

Data-driven reevaluation of f t values in superallowed β decays

We present a comprehensive reevaluation of the ft values in superallowed nuclear β decays crucial for the precise determination of V ud and low-energy tests of the electroweak standard model. It consists of the first, fully data-driven analysis of the nuclear β decay form factor, that utilizes isospin relations to connect the nuclear charged weak distribution to the measurable charge distributions. This prescription supersedes previous shell-model estimations, and allows for a rigorous quantification of theory uncertainties in f which is absent in the existing literature. Furthermore, our new evaluation shows an overall downward shift of the central values of f at the level of 0.01%.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2022

Impact of Clustering on the Li 8 β Decay and Recoil Form Factors

We place unprecedented constraints on recoil corrections in the β decay of 8 Li, by identifying a strong correlation between them and the 8 Li ground state quadrupole moment in large-scale ab initio calculations. The results are essential for improving the sensitivity of high-precision experiments that probe the weak interaction theory and test physics beyond the standard model. In addition, our calculations predict a 2 + state of the α + α system that is energetically accessible to β decay but has not been observed in the experimental 8 Be energy spectrum, and has an important effect on the recoil corrections and β decay for the A = 8 systems. Furthermore, this state and an associated 0 + state are notoriously difficult to model due to their cluster structure and collective correlations, but become feasible for calculations in the ab initio symmetry-adapted no-core shell-model framework.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2026

A Physics-Aligned Multi-Domain Machine Learning Framework for Time-Localised Diagnosis of Power Electronics Faults

This paper presents a physics-aligned framework for fault diagnosis in multi-phase power-electronic systems using cycle-synchronous windowing and multi-domain features derived from Fourier, wavelet, and Hilbert–Huang representations. While both logistic regression and multilayer perceptron (MLP) models achieve perfect performance under standard evaluation, blind unseen testing reveals a critical failure in a baseline MLP. This is shown to arise from model selection based on validation accuracy. Using validation-loss-based selection restores correct unseen performance and improves confidence. Feature ablation shows that Fourier and wavelet features dominate, while computational analysis indicates that feature extraction, particularly HHT, governs runtime.

Kumar, Praveen [ORNL] (ORCID:0000000291877857)↗
DOE OSTI2025

Uniform Mechanical Loading Can Test for Nonuniform Loading Durability

In this work, we present a method to evaluate the equivalency between any module mechanical loading conditions. The method is developed to address the specific failure mode of glass fracture and is based on Weibull analysis and weakest link theory. It considers the varying stress profile across the module to calculate the probability of glass fracture, which is used as the metric of equivalency. An idealized nonuniform loading scheme is employed to demonstrate the method and introduce the concept of the equivalent uniform load factor: a factor applied to the maximum pressure of the nonuniform load to obtain the equivalent uniform load value. It is demonstrated that this factor is less than unity for all nonuniform load cases considered, including snow and various characters of wind loading. These significant results suggest that uniform loading may be reliably, and practically, employed to evaluate photovoltaic module glass for nonuniform loading durability.

14 SOLAR ENERGY↗
DOE OSTI2026

Surface Stress Characterization and Trends in Thermally Strengthened Photovoltaic Module Glass

Simultaneous changes in photovoltaic (PV) module architecture-such as increased area, replacing the polymeric backsheet with a glass backsheet, and reducing glass thickness from 3.2 to 2.0 mm-have resulted in a novel failure called spontaneous glass breakage. Spontaneous glass breakage results in front and/or rear glass failure without any obvious cause. The resulting low-energy fracture patterns have raised concerns about the thermal strengthening in 2.0-mm glass. We present validation of a nondestructive method for measuring the glass surface stress in PV modules. We use a scattered light polariscope to examine the glass properties of 11 modules from 6 solar fields, with and without spontaneous glass breakage. Based on a Mann-Whitney test p-value of 1.4 x 10-6, we conclude that there is a correlation between lower surface stress and susceptibility to spontaneous breakage. A Kendall's Tau test p-value of 2.0 x 10-4 indicates a correlation between increased module area and lower surface stress. We find that 2.0-mm glass can be, and often is, fully tempered (surface stress ≥69 MPa), but inspecting the fracture pattern is not a reliable way to assess the amount of thermal strengthening. A combination of factors, not just surface stress, influences glass breakage.

14 SOLAR ENERGY↗
DOE OSTI2026

Different Damp-Heat-Induced Series Resistance Degradation Behaviors in Fielded Crystalline Silicon Photovoltaic Modules Due to Difference in Bill of Materials

This case study investigates mono-crystalline silicon modules from underperforming portions of a utility-scale photovoltaic power plant. Field-collected I-V curves and electroluminescence imaging suggested that increased series resistance was a primary factor driving module degradation. Selected modules were removed from the field for further analysis, including incremental damp heat accelerated testing, which confirmed a progression in series resistance degradation. Two distinct cell degradation behaviors became apparent during the investigation. Cross-sectional scanning electron microscopy (with elemental analysis) and scanning spreading resistance microscopy identified key differences between the two degradation mechanisms, primarily grid finger width and contact resistance. Additionally, the study highlights the reliability implications of retest requirements in International Electrotechnical Commission 61215 for material changes and how they may have mitigated the degradation observed at this site.

14 SOLAR ENERGY↗
DOE OSTI2020

On the Computational Viability of Quantum Optimization for PMU Placement

Using optimal phasor measurement unit placement as a prototypical problem, we assess the computational viability of the current generation D-Wave Systems 2000Q quantum annealer for power systems design problems. We reformulate minimum dominating set for the annealer hardware, solve the reformulation for a standard set of IEEE test systems, and benchmark solution quality and time to solution against the CPLEX optimizer and simulated annealing. For some problem instances the 2000Q outpaces CPLEX. For instances where the 2000Q underperforms with respect to CPLEX and simulated annealing, we suggest hardware improvements for the next generation of quantum annealers.

hardware↗
DOE OSTI2022

Training data selection for event classification in a highly variable environment

A problem of interest for nuclear nonproliferation is monitoring activities at nuclear facilities, where proliferation events may only take place a few times and often under variable conditions. Machine learning has revolutionized data analytics by enabling the use of measurable signatures to generate predictive models of facility operations. However, traditional methods for training these models require large, reliable data sets with labeled observations, a challenge for nonproliferation. Highly variable conditions further complicate this as events from training data may have occurred in conditions quite different from the event of interest. Our hypothesis is that when events occur in a highly variable environment, careful training data selection for each test event could outperform the standard approach of using all available training data. We developed a method to optimize training data selection for the given test event and applied it to predicting the power level of the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory. In this study, the reactor startup exhibits variability between occurrences due to natural variability in environmental conditions and operational procedures. Using a combination of analysis techniques, a similitude assessment was performed on data collected from HFIR to isolate clusters that were optimal for training a predictive model. Concepts such as dynamic time warping and Jaccard similarity were used in conjunction with clustering analysis. In order to validate this approach, the model was trained on every combination of unique training events and the predictive performance was compared to the performance using a subset of the training data selected by isolated clusters found through the similitude assessment.

Iyer, A↗
DOE OSTI2022

Converter-Interfaced CHP Plant for Improved Grid-Integration, Flexibility and Resiliency

GE Research and its partner GE Renewables have proposed the use of an interface converter solution to increase the penetration of small to medium-sized CHP (1MWe to 20MWe) into distribution grids and improve their flexibility and grid support capability. Indeed, the proposed interface converter solution thanks to presence of the grid-ready inverter, allows to streamline the compliance to grid codes requirements, reduce the interconnection delays and costs and ultimately one of the main barriers for CHP adoption by commercial and industrial facilities. An additional benefit provided by the interface converter is the use of the grid-ready inverter for reactive power which eliminates the need of sizing the generator for that capability. These two benefits highly favor the economic feasibility of converter-interfaced CHP. Five user cases, each in one of the leading U.S states for CHP potential reported by the DOE in its estimation of the U.S Technical Potential of CHP, were selected to compare the economic performances of converter-interfaced CHP as compared with directly-coupled. They include a college campus in California, a hospital in New York, a water reclamation plant in Texas, a hotel in Minnesota, and a large office building in Pennsylvania. Results showed that, the presence of the interface converter allows to increase the return on investment (ROI) by 0.5 to 2 percentage points in most of the cases (4 of 5). Indeed, the interface converter by shortening the interconnection process allows to accelerate revenues while reducing interconnection costs. Added to the reduced cost of the required generator these savings trade favorably the capital cost of the converter. The analysis also showed that the profitability of the converter-interfaced CHP is highly sensitive to the energy price, interconnection delay, and converter cost. However, it appears that if the interface converter can shorten the interconnection process by at least 6 months, adopting this solution will be more economically viable than directly-coupled configuration in almost all the +23,000 sites of the U.S Technical Potential CHP. The evaluation of the benefits of a converter-interfaced CHP also showed that it enables higher ROI when coupled with other distributed energy resources (DER) such as battery energy systems (BESS) or solar photovoltaic (PV). Indeed, in those scenario, the grid-ready inverter included in the interface converter eliminates the need of separate inverters if DC-coupling is used. On the technical performance, it has been verified that the presence of the interface converter allows to reduce by 70% to 80% the CHP short-circuit contribution to grid faults. This not only reduces the mechanical and thermal stresses exposed to the CHP electrical components but also increases the grid hosting capacity which ultimately enables higher penetrations CHP. Another key benefit of the interface converter validated with hardware-in-the-loop simulations and testing is its superior capability for reactive power support. Indeed, using a power hardware testbed with two +700kW inverters configured in back-to-back, a microgrid controller and actual facilities loads it was demonstrated that the presence of the interface converter can help maintain a power factor near ~1 or regulate the voltage to ~1.0pu at the point of common coupling. This benefit can be highly valuable if in the future, due to higher penetration of renewable distributed energy resources (DER), utilities start billing demand charge based on kVA instead of kW as currently. It was also validated that converter-interfaced CHP can dispatch heat and power commands and seamlessly switch between the two modes while consistently controlling the power factor or voltage at PCC. Indeed, the power hardware testing showed that grid-connected converter-interfaced CHP can follow either the power or heat demand while maintaining a unity power factor at converter output. This research proved that the adoption of an interface converter as the solution for interconnection of CHP system into the distribution grid can greatly improve the economic feasibility of small to medium-sized CHP as well as the plant power quality, flexibility and resiliency. Additionally, it allows increased penetrations of CHP into the distribution grid, extends their grid support capability, and facilitates the integration of BESS and PV DER by streamlining their collocation within the same facilities. This ultimately provides an opportunity for commercial and small industrial facilities in the U.S to accelerate their energy transition thanks to the high energy efficiency of CHP systems and its reliable, flexible, and resilient microgrid operation when interconnected with an interface converter.

24 POWER TRANSMISSION AND DISTRIBUTION↗
DOE OSTI2024

Standards Guidance for Electric Two- and Three-Wheelers and Charging Infrastructure in Pakistan

Electric two-wheelers (E2Ws) and electric three-wheelers (E3Ws) have reached upfront cost price parity as compared to their conventional counterparts in many markets (IEA 2022). Therefore, Pakistan has embraced E2Ws and E3Ws in their National Electric Vehicle Policy (Government of Pakistan 2019b). Specifically, this policy targets 50% of new two- and three-wheeler sales to be electric by 2030. In the short term, this policy targets five times as many E2Ws and E3Ws as cars, vans, and pickups. In order to meet these goals in a safe, reliable, and efficient manner, Pakistan needs to develop and implement standards related to E2W and E3W vehicles and charging infrastructure, including battery swap stations. Without standards, E2Ws and E3Ws can be dangerous, unreliable, incompatible with charging stations, or diminish the grid’s electricity quality (Goel and Singh 2019; Sasidharan 2020). Fortunately, there are several global and local efforts to establish standards that Pakistan can learn from or adopt. This document explains the purpose and process of standards development and introduces the international standards development organizations involved and relevant classification and testing systems. It then introduces and lists many standards related to the vehicles, batteries, and charging equipment so that Pakistan can adopt or reference these standards when developing its own.

33 ADVANCED PROPULSION SYSTEMS↗
DOE OSTI2025

Using Separation-Enhanced Isotope Ratio Mass Spectrometry to Enable Increased Renewable Carbon Content in Transportation Fuels (CRADA 525)

Stable isotope ratio measurements of carbon atoms using isotope ratio mass spectrometry (IRMS) can be an effective tool for quantifying biogenic carbon in co-processed fuels, with results approaching the precision and accuracy of accelerator mass spectrometry (AMS). The lower cost of an IRMS may enable deployment to refineries, improving access and analysis turnaround times (≤2 hours), and, by extension, provide data that can allow process optimization to maximize renewable carbon in desired refinery products. This project explored the integration of chemical separation with IRMS analyses to enable highly detailed tracking of biogenic carbon into fuel product streams separated by boiling point range, chemical class, or specific compound. Forty-nine fuels and fuel components of fossil and biogenic origin, spanning gasoline and diesel boiling point ranges, were received from three refiners and were analyzed for their δ 13 C values via IRMS. Results spanned a 13 C range from ca. 10‰ to 44‰ and reflect materials derived from sustainable sources (e.g., C4 or C3 plants, animal-based pathways, syngas) or from fossil-derived fuels. Common ranges are approximately 18‰ to 9‰ and approximately 30‰ to 20‰ for C4 and C3 plants, respectively, and approximately 34‰ to 24‰ and approximately 70‰ to 33‰ for petroleum-derived fuels and methane, respectively. Fuel-like standards were developed and tested using direct-injection elemental analyzer (EA) IRMS for liquid fuels. This method was compared with the published methods, yielding statistically similar results. Four blend curve sets were produced ranging from 0% to 100% of a fuel containing biogenic carbon, focusing on 0% to 10% biogenic carbon. Linear fits were the most applicable for two of the four blend curve sets; however, two sets were found to exhibit slightly quadratic behavior, which was more pronounced in low biogenic blend samples, necessitating second-order fits. The origin of the slight quadratic behavior remains unclear; however, the discussion points to possible interpretations. CanmetENERGY thoroughly characterized a majority of the samples using one- and two-dimensional gas chromatography (GC and GC×GC, respectively) and other analyses. Selected samples were subjected to solid phase extraction (SPE) for saturate, olefin, aromatic, and polar (SOAP) analysis, and the resulting solvent-diluted fractions containing saturates and aromatics were returned to Pacific Northwest National Laboratory (PNNL), where the solvent was removed via evaporation or physical separation using GC techniques. Characterization and separations provided an understanding of saturate and aromatic content, as well as boiling point ranges for each sample and sample fraction. Samples resulting from SPE were examined using EA-IRMS and gas chromatography combustion IRMS (GC-C-IRMS) analyses. Both approaches suggest that the range in values between end-members can be increased by selecting the paraffinic or aromatic fraction of the end-member or by selecting among individual compounds resulting from GC separation of the paraffinic fractions. Considerable work remains to put these approaches into practice and statistically validate the benefit for using a fraction or individual compound over bulk analysis of a sample. However, initial results suggest that separations provide advantages for samples having blend ratios of less than 10% biogenic blendstocks. 13 C results showed statistically similar biofuel blend results to those obtained at PNNL, although additional work is needed to obtain better reproducibility. Select samples were sent to Los Alamos National Laboratory (LANL) for IRMS measurements and Beta Analytics for AMS measurements. This work suggests that IRMS and AMS yield closely comparable results and in some circumstances, IRMS could serve as a surrogate for AMS. While additional work is needed to better resolve statistical advantages for separations and better show the comparable nature of IRMS and AMS in both the biogenic carbon analysis of bulk chemical classes, initial results from this study suggest that these should be pursued in order to proliferate this approach for quantifying biogenic carbon in transportation fuels to the refinery level, thereby potentially enabling process optimization in co-processing scenarios.

09 BIOMASS FUELS↗