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DOE OSTI2025

Challenges and strategies for probing the composite interface of PEM electrolyzers and fuel cells using operando AP-XPS

Left: cross-section schematic of a membrane electrode assembly, the working electrode changing state with applied potential. Center: the operando cell design that enables snapshot data acquisition during trajectory movement. Right: resulting spectra. Understanding the surface chemistry of electrocatalyst systems under operando conditions is central to revealing the electrocatalytic cell's working mechanisms. Determination of these catalytic processes on a molecular scale and the involved components is fundamental to streamlining material design for energy conversion and storage applications. X-ray photoelectron spectroscopy (XPS) is an established technique used to study the chemical and electronic states of materials. While the surface sensitivity of XPS is typically high, use of tender X-ray energies and technical advancements have allowed for the direct probing of solid–vapor and solid–liquid interfaces. However, protocols and documentation of experimental considerations for operando XPS probing of working electrolyzers and fuel cells remain scarce. Herein, we report an approach for the study of working polymer electrolyte membrane (PEM) electrolysis cells using ambient pressure X-ray photoelectron spectroscopy (AP-XPS). This approach directly probes the composite electrode surface on the membrane electrode assembly (MEA) in 100% relative humidity to establish a meaningful liquid layer for electrocatalysis. We carry out a systematic investigation from the cell constituent components to a fully assembled working operando electrolytic system and establish a method for AP-XPS study of the complex composite MEA, providing recommendations for data acquisition and component analysis.

Hamlyn, Rebecca↗

DOE OSTI2014

A protocol for lifetime energy and environmental impact assessment of building insulation materials

This article describes a proposed protocol that is intended to provide a comprehensive list of factors to be considered in evaluating the direct and indirect environmental impacts of building insulation materials, as well as detailed descriptions of standardized calculation methodologies to determine those impacts. The energy and environmental impacts of insulation materials can generally be divided into two categories: (1) direct impact due to the embodied energy of the insulation materials and other factors and (2) indirect or environmental impacts avoided as a result of reduced building energy use due to addition of insulation. Standards and product category rules exist, which provide guidelines about the life cycle assessment (LCA) of materials, including building insulation products. However, critical reviews have suggested that these standards fail to provide complete guidance to LCA studies and suffer from ambiguities regarding the determination of the environmental impacts of building insulation and other products. The focus of the assessment protocol described here is to identify all factors that contribute to the total energy and environmental impacts of different building insulation products and, more importantly, provide standardized determination methods that will allow comparison of different insulation material types. Further, the intent is not to replace current LCA standards but to provide a well-defined, easy-to-use comparison method for insulation materials using existing LCA guidelines. - Highlights: • We proposed a protocol to evaluate the environmental impacts of insulation materials. • The protocol considers all life cycle stages of an insulation material. • Both the direct environmental impacts and the indirect impacts are defined. • Standardized calculation methods for the ‘avoided operational energy’ is defined. • Standardized calculation methods for the ‘avoided environmental impact’ is defined.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2022

Standardized protocols for evaluating platinum group metal-free oxygen reduction reaction electrocatalysts in polymer electrolyte fuel cells

Platinum group metal (PGM)-free electrocatalysts for the oxygen reduction reaction at the polymer electrolyte fuel cell cathode have shown substantial improvements in activity—especially those derived from transition metals, nitrogen and carbon. However, their stability and durability remain insufficient. A key to enabling future improvements and performance comparisons lies in the development of test protocols that are relevant to the operating conditions of the fuel cell cathode, can be completed within a reasonable time and are ubiquitously adopted. Here we propose and validate such protocols, designed with special attention to typical catalyst degradation mechanisms of PGM-free catalysts. The results of the cross-laboratory validation study using two different catalysts attest to the strength and feasibility of the proposed approach. We hope that the information provided here can serve as a broad and effective platform for assessing the performance and durability of PGM-free catalysts for polymer electrolyte fuel cells.

25 ENERGY STORAGE↗

DOE OSTI2023

Best practices in NMR metabolomics: Current state

A literature survey was conducted to identify current practices used by NMR metabolomics investigators when conducting and reporting their metabolomics studies. A total of 463 papers from 2020 and 80 papers from 2010 were selected from PubMed and were manually analyzed by a team of investigators to assess the extent and completeness of the experimental procedures and protocols reported. A significant number of the papers did not report on essential experimental details, incompletely stated which statistical methods were used, improperly applied supervised multivariate statistical analyses, or lacked validation of statistical models. A large diversity of protocols and software were identified, which suggests a lack of consensus and a relatively limited use of commonly agreed upon standards for conducting and reporting NMR metabolomics studies. In conclusion, the overall intent of the survey is to inform and encourage the NMR metabolomics community to develop and adopt best-practices for the field.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

GeoRePORT Case Study Examples: Reporting Using the Geothermal Resource Portfolio Optimization and Reporting Technique (GeoRePORT)

The Geothermal Research Portfolio Optimization & Reporting Technique (GeoRePORT) was developed with funding from the United States Department of Energy's Geothermal Technologies Office (GTO) to assist in identifying and pursuing long-term investment strategies through the development of a resource reporting protocol. GeoRePORT provides scientists and non-scientists a comprehensive and quantitative means of reporting: (1) features intrinsic to geothermal sites (project grade) and, (2) maturity of the development (project readiness). Because geothermal feasibility is not determined by any single factor (e.g. temperature, permeability, permitting), a site's project grade and readiness are evaluated on twelve independent attributes pertaining to geological, technical, or socio-economic feasibility. In this paper, we present case studies illustrating how GeoRePORT can be used to compare geological, technical, and socio-economic attributes between geothermal systems. The consistent and objective assessment protocols used in GeoRePORT allow for comparison of project attributes across unique locations and geological settings. GeoRePORT case studies outline the geological, socio-economic and technical features of four individual geothermal sites: Coso, Chena, Dixie Valley, and White Sands Missile Range. The case studies presented herein illustrate the usefulness of GeoRePORT in evaluating project risk/return, identifying gaps in reported data, evaluating R&D impact, and gathering insights on successes/failures as applicable to future projects.

40 EE - Geothermal Technologies Office (EE-4G)↗

DOE OSTI2024

A Simulation Study of Quantum Clock Synchronization Using Teleportation

An important requirement in implementing distributed computing and sensing application is the synchronization of clocks at various locations. The Internet relies on the Network Time Protocol (NTP), which synchronizes clocks with accuracy in the order of milliseconds. More recently an ensemble of atomic clocks is used for navigation based on GPS. These clocks are highly accurate and provide time with very low uncertainty. Even so, many physics experiments such as distributed LIGO-based systems may require more accurate clock synchronization that is achievable using quantum entanglement. This requires the deployment of a network of quantum clocks synchronized by exploiting entangled atomic clock qubits. In this paper, we carry out a simulation study of synchronizing a network of quantum clocks interconnected by a fiber plant that supports the ESnet; the latter is used to support the classical communication needed for teleportation. We consider an existing protocol for synchro-nizing the atomic clock qubits that relies on the GHZ states. To assess the performance of the protocol we developed a discrete-event simulation of the network using IBM Qiskit framework for underlying quantum gate operations and measurements. The simulation results shed light on the resources required in terms of the number entangled qubits and the time needed to achieve the synchronization of different number of nodes in ESnet.

Kiran, Mariam↗

NASA NTRS1994

The development and application of composite complexity models and a relative complexity metric in a software maintenance environment

A great deal of effort is now being devoted to the study, analysis, prediction, and minimization of software maintenance expected cost, long before software is delivered to users or customers. It has been estimated that, on the average, the effort spent on software maintenance is as costly as the effort spent on all other software costs. Software design methods should be the starting point to aid in alleviating the problems of software maintenance complexity and high costs. Two aspects of maintenance deserve attention: (1) protocols for locating and rectifying defects, and for ensuring that noe new defects are introduced in the development phase of the software process; and (2) protocols for modification, enhancement, and upgrading. This article focuses primarily on the second aspect, the development of protocols to help increase the quality and reduce the costs associated with modifications, enhancements, and upgrades of existing software. This study developed parsimonious models and a relative complexity metric for complexity measurement of software that were used to rank the modules in the system relative to one another. Some success was achieved in using the models and the relative metric to identify maintenance-prone modules.

Hops, J. M.↗

DOE OSTI2019

GeoRePORT Case Study Examples: Reporting Using the Geothermal Resource Portfolio Optimization and Reporting Technique (GeoRePORT): Preprint

15 GEOTHERMAL ENERGY↗

DOE OSTI2013

A gEUD-based inverse planning technique for HDR prostate brachytherapy: Feasibility study

Purpose: The purpose of this work was to study the feasibility of a new inverse planning technique based on the generalized equivalent uniform dose for image-guided high dose rate (HDR) prostate cancer brachytherapy in comparison to conventional dose-volume based optimization. Methods: The quality of 12 clinical HDR brachytherapy implants for prostate utilizing HIPO (Hybrid Inverse Planning Optimization) is compared with alternative plans, which were produced through inverse planning using the generalized equivalent uniform dose (gEUD). All the common dose-volume indices for the prostate and the organs at risk were considered together with radiobiological measures. The clinical effectiveness of the different dose distributions was investigated by comparing dose volume histogram and gEUD evaluators. Results: Our results demonstrate the feasibility of gEUD-based inverse planning in HDR brachytherapy implants for prostate. A statistically significant decrease in D{sub 10} or/and final gEUD values for the organs at risk (urethra, bladder, and rectum) was found while improving dose homogeneity or dose conformity of the target volume. Conclusions: Following the promising results of gEUD-based optimization in intensity modulated radiation therapy treatment optimization, as reported in the literature, the implementation of a similar model in HDR brachytherapy treatment plan optimization is suggested by this study. The potential of improved sparing of organs at risk was shown for various gEUD-based optimization parameter protocols, which indicates the ability of this method to adapt to the user's preferences.

60 APPLIED LIFE SCIENCES↗

NASA NTRS2016

Influence of Measurement Uncertainties on Fractional Solubility of Iron in Mineral Aerosols over the Oceans

The atmospheric supply of mineral dust iron (Fe) plays a crucial role in the Earths biogeochemical cycle and is of specific importance as a micronutrient in the marine environment. Observations show several orders of magnitude variability in the fractional solubility of Fe in mineral dust aerosols, making it hard to assess the role of mineral dust for the global ocean biogeochemical Fe cycle. In this study we compare the operational solubility of mineral dust aerosol Fe associated with the flow-through leaching protocol to the results of the global 3-D chemical transport model GEOS-Chem. According to the protocol, aerosol Fe is defined as soluble by first deionized water leaching of mineral dust through a 0.45 m pore size membrane followed by acidification and storage of the leachate over a long period of time prior to analysis. To estimate the uncertainty in soluble Fe results introduced by the flow-through leaching protocol, we prescribe an average 50 (range of 30 to 70) fractional solubility to sub-0.45 m sized mineral dust particles that may inadvertently pass the filter and end up in the acidified (at pH1.7) leachate for a couple of month period. In the model, the fractional solubility of Fe is either explicitly calculated using a complex mineral aerosol Fe dissolution module, or prescribed to be 1 and 4. Calculations show that the fractional solubility of Fe derived through the flow-through leaching is higher compared to the model results. The largest differences (40) are predicted to occur farther away from the dust source regions, over the areas where sub-0.45 m sized mineral dust particles contribute a larger fraction of the total mineral dust mass. This study suggests that different methods used in soluble Fe measurements and inconsistences in the operational definition of filterable Fe in marine environment and soluble Fe in atmospheric aerosols are likely to contribute to the wide range of fractional solubility of aerosol Fe reported in the literature.

Soluble Iron↗

DOE OSTI2016

Model sensitivity studies of the decrease in atmospheric carbon tetrachloride

Carbon tetrachloride (CCl 4 ) is an ozone-depleting substance, which is controlled by the Montreal Protocol and for which the atmospheric abundance is decreasing. But, the current observed rate of this decrease is known to be slower than expected based on reported CCl 4 emissions and its estimated overall atmospheric lifetime. Here we use a three-dimensional (3-D) chemical transport model to investigate the impact on its predicted decay of uncertainties in the rates at which CCl 4 is removed from the atmosphere by photolysis, by ocean uptake and by degradation in soils. The largest sink is atmospheric photolysis (74 % of total), but a reported 10 % uncertainty in its combined photolysis cross section and quantum yield has only a modest impact on the modelled rate of CCl 4 decay. This is partly due to the limiting effect of the rate of transport of CCl 4 from the main tropospheric reservoir to the stratosphere, where photolytic loss occurs. The model suggests large interannual variability in the magnitude of this stratospheric photolysis sink caused by variations in transport. The impact of uncertainty in the minor soil sink (9 % of total) is also relatively small. In contrast, the model shows that uncertainty in ocean loss (17 % of total) has the largest impact on modelled CCl 4 decay due to its sizeable contribution to CCl 4 loss and large lifetime uncertainty range (147 to 241 years). Furthermore, with an assumed CCl 4 emission rate of 39 Gg year -1 , the reference simulation with the best estimate of loss processes still underestimates the observed CCl 4 (overestimates the decay) over the past 2 decades but to a smaller extent than previous studies. Changes to the rate of CCl 4 loss processes, in line with known uncertainties, could bring the model into agreement with in situ surface and remote-sensing measurements, as could an increase in emissions to around 47 Gg year -1 . Further progress in constraining the CCl 4 budget is partly limited by systematic biases between observational datasets. For example, surface observations from the National Oceanic and Atmospheric Administration (NOAA) network are larger than from the Advanced Global Atmospheric Gases Experiment (AGAGE) network but have shown a steeper decreasing trend over the past 2 decades. The observed differences imply a difference in emissions which is significant relative to uncertainties in the magnitudes of the CCl 4 sinks.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2016

SU-G-TeP2-01: Can EPID Based Measurement Replace Traditional Daily Output QA On Megavoltage Linac?

Purpose: To investigate the long term stability and viability of using EPID-based daily output QA via in-house and vendor driven protocol, to replace conventional QA tools and improve QA efficiency. Methods: Two Varian TrueBeam machines (TB1&TB2) equipped with electronic portal imaging devices (EPID) were employed in this study. Both machines were calibrated per TG-51 and used clinically since Oct 2014. Daily output measurement for 6/15 MV beams were obtained using SunNuclear DailyQA3 device as part of morning QA. In addition, in-house protocol was implemented for EPID output measurement (10×10 cm fields, 100 MU, 100cm SID, output defined over an ROI of 2×2 cm around central axis). Moreover, the Varian Machine Performance Check (MPC) was used on both machines to measure machine output. The EPID and DailyQA3 based measurements of the relative machine output were compared and cross-correlated with monthly machine output as measured by an A12 Exradin 0.65cc Ion Chamber (IC) serving as ground truth. The results were correlated using Pearson test. Results: The correlations among DailyQA3, in-house EPID and Varian MPC output measurements, with the IC for 6/15 MV were similar for TB1 (0.83–0.95) and TB2 (0.55–0.67). The machine output for the 6/15MV beams on both machines showed a similar trend, namely an increase over time as indicated by all measurements, requiring a machine recalibration after 6 months. This drift is due to a known issue with pressurized monitor chamber which tends to leak over time. MPC failed occasionally but passed when repeated. Conclusion: The results indicate that the use of EPID for daily output measurements has the potential to become a viable and efficient tool for daily routine LINAC QA, thus eliminating weather (T,P) and human setup variability and increasing efficiency of the QA process.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2024

A Semi‐Automated, High‐Throughput Approach for the Synthesis and Identification of Highly Photo‐Cytotoxic Iridium Complexes

Abstract The discovery of new compounds with pharmacological properties is usually a lengthy, laborious and expensive process. Thus, there is increasing interest in developing workflows that allow for the rapid synthesis and evaluation of libraries of compounds with the aim of identifying leads for further drug development. Herein, we apply combinatorial synthesis to build a library of 90 iridium(III) complexes (81 of which are new) over two synthesise‐and‐test cycles, with the aim of identifying potential agents for photodynamic therapy. We demonstrate the power of this approach by identifying highly active complexes that are well‐tolerated in the dark but display very low nM phototoxicity against cancer cells. To build a detailed structure–activity relationship for this class of compounds we have used density functional theory (DFT) calculations to determine some key electronic parameters and study correlations with the experimental data. Finally, we present an optimised semi‐automated synthesise‐and‐test protocol to obtain multiplex data within 72 hours.

Kench, Timothy↗

DOE OSTI2024

A Semi‐Automated, High‐Throughput Approach for the Synthesis and Identification of Highly Photo‐Cytotoxic Iridium Complexes

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Say where you sample: Increasing site selection transparency in urban ecology

Urban ecological studies have the potential to extend our understanding of socio-ecological systems beyond that of an individual city or region. Cross-comparative empirical work and synthesis are imperative to develop a general urban ecological theory. This can be achieved only if studies are replicable and generalizable. Transparency in methods reporting facilitates generalizability and replicability by documenting the decisions scientists make during the various steps of research design; this is particularly true for sampling design and selection because of their impact on both internal and external validity and the potential to unintentionally introduce bias. Three interdependent aspects of sample design are study sample selection (e.g., specific organisms, soils, or water), sample specification (measurement of specific variable of interest), and site selection (locations sampled). Of these, documentation of site selection—the where component of sample design—is underrepresented in the urban ecology literature. Using a stratified random sample of 158 papers from 12 major urban ecology journals, we investigated how researchers selected study sites in urban ecosystems and evaluated whether their site selection methods were transparent. We extracted data from these papers using a 50-question, theory-based questionnaire and a multiple-reviewer approach. Our sample represented almost 45 years of urban ecology research across 40 different countries. We found that more than 80% of the papers read were not transparent in their site selection methodology. We do not believe site selection methods are replicable for 70% of the papers read. Key weaknesses include incomplete descriptions of populations and sampling frames, urban gradients, sample selection methods, and property access. Low transparency in reporting the where methodology limits urban ecologists’ ability to assess the internal and external validity of studies’ findings and to replicate published studies; it also limits the generalizability of existing studies. The challenges of low transparency are particularly relevant in urban ecology, a field where standard protocols for site selection and delineation are still being developed. These limitations interfere with the fields’ ability to build theory and inform policy. We conclude by offering a set of recommendations to increase transparency, replicability, and generalizability.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2019

Ab initio thermal rate coefficients for H + NH 3 ⇌ H 2 + NH 2

The reversible reaction NH 3 + H ⇌ H 2 + NH 2 , which plays an important role in NH3 fuel combustion, is studied with a theoretical approach that combines the high-accuracy extrapolated ab initio thermochemistry (HEAT) protocol with semiclassical transition state theory (SCTST). The calculated forward reaction is endothermic by 11.8 ± 1 kJ/mol, in nearly perfect agreement with the active thermochemical tables (ATcT) value of 11.5 ± 0.2 kJ/mol. Using this improved thermochemistry yields better rate constants, especially at low temperatures. Experimental rate constants available from 400 to 2000 K for the forward and reverse reaction pathways can be reproduced (within 20%) by the calculations from first principles.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2019

Upper urinary tract urothelial carcinoma on multidetector CT: spectrum of disease

Urothelial carcinoma of the upper urinary tract (UUT) is a relatively uncommon genitourinary malignancy, accounting for about 5–7% of urothelial tumors. The significant features of this tumor are multifocality and high rate of recurrence. Computed tomography urography (CTU) has replaced excretory urography (EU) and retrograde pyelography (RP) for imaging of upper tract urothelial carcinoma. While many studies have confirmed high sensitivity (88–100%) and specificity (93–100%) of CTU, an optimized CT protocol is of critical importance in screening, staging, and post-operative follow-up of patients (Chlapoutakis, Eur J Radiol 73(2):334–338, 2010; Caoli and Cohan, Abdom Radiol (NY) 41(6):1100–1107, 2016). The key element of the CT protocol is to have adequate distension of the collecting system with excreted contrast, to detect subtle lesions at an early stage. In this article, we discuss the background of upper urinary tract TTC, pathogenesis, CT protocol and the role of imaging in evaluation of this malignancy, staging, as well as different imaging appearances.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

DOE OSTI2015

Degradation of transparent conductive oxides: Interfacial engineering and mechanistic insights

Transparent conductive oxides (TCOs) are a known failure mode in a variety of thin film photovoltaic (PV) devices, through mechanisms such as resistivity increase and delamination. Degradation science studies of these materials, as well as most PV systems, have primarily utilized industry standard qualification protocols, which are not designed to be used as lifetime prediction tests. Here, this work applies a data science approach to this engineering challenge, utilizing commercially available TCOs and subjecting them to an array of stressors, including environmental and material stressors. Optical, electrical and surface sensitive TCO property metrics were monitored and analyzed en mass. Different degradation mechanisms and modes were observed when different stressor combinations were applied; TCO surfaces are sensitive to the proportion of water and light in an exposure, yellowing of the TCO only occurs when humidity and UV light are combined, and PEDOT:PSS (poly(3,4-ethylenedioxythiophene) poly(styrenesulfonate)) application results in hazing and roughening of aluminum-doped zinc oxide (AZO). Using multi-variate analytics and plotting critical material properties against one another in a mechanistic plot, trade-offs between properties and the activation of different degradation mechanisms become readily apparent. In addition to a survey of failure modes of TCOs, a possible solution to the degradation of AZO was examined: the application of an organofunctional silane layer. The application of a thin APTES (3-aminopropyltriethoxysilane) film nearly eliminated the observed edge effects and greatly reduced the resistivity increase caused by damp heat exposure of AZO.

14 SOLAR ENERGY↗