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NASA NTRS2000

Tenth AMS Conference on Satellite Meteorology and Oceanography

The American Meteorological Society held its Tenth Conference on Satellite Meteorology and Oceanography in conjunction with the 80th Annual Meeting in Long Beach, California. For the second consecutive conference, a format that consisted of primarily posters, complemented by invited theme oriented oral presentations, and panel discussions on various aspects on satellite remote sensing were utilized. Joint sessions were held with the Second Conference on Artificial Intelligence, the Eleventh Conference on Middle Atmosphere, and the Eleventh symposium on Global Change Studies. In total, there were 23 oral presentations, 170 poster presentations, and four panel discussions. Over 450 people representing a wide spectrum of the society attended one or more of the sessions in the five-day meeting. The program for the Tenth Conference on Satellite Meteorology and Oceanography can viewed in the October 1999 issue of the Bulletin.

Ferraro, R.↗
NASA NTRS2002

A Downscaling Analysis of the Urban Influence on Rainfall: TRMM Satellite Component AMS Conference on Satellite Meteorology and Oceanography

A recent publication by Shepherd et al. (2002) demonstrated the feasibility of using TRMM precipitation radar (PR) estimates to identify precipitation anomalies caused by urbanization. The approach is particularly useful for investigating this global process because TRMM data span large portions of the globe and comprise an extended temporal dataset. Recent literature suggests that urbanized regions of Houston, Texas may be influencing lightning and precipitation formation over and downwind of the city. Possible mechanisms include: (1) enhanced convergence through interactions between the sea breeze, Galveston bay breeze, and urban heat island circulations, (2) enhanced convergence due to increased surface roughness over the city and/or destabilization of the boundary layer by the UHI, or (3) enhanced cloud condensation nuclei due to urban and industrial aerosol sources. In this study, a downscaling analysis of spatial and temporal trends in rainfall around the Houston Area is being conducted. The downscaling analysis concept involves identifying and quantifying urban rainfall anomalies at progressively smaller spatial and temporal scales using the TRMM satellite, ground-based radar, and a dense network of rain gauges. The goal is to test the hypothesis that the Houston urban district and regions in the climatological downwind region of the city exhibit enhanced rainfall amounts relative to the climatological upwind regions. TRMM was launched in 1997 and currently operates in a low-inclination (35 deg), non-sun-synchronous orbit at an altitude of 402 km (350 km prior to August 2001). The satellite analysis follows the methodologies described in Shepherd et al. (2002). Nearly five years of TRMM PR-derived mean monthly rainfall estimates are utilized to produce annual and warm season isohyetal analyses around Houston. Early results indicate that rainfall rates (mm/h) for the entire period are largest within 100 km northeast and east of Houston (e.g. the "hypothesized downwind region"). The mean rainfall rate over the Houston urban center is 30.5% larger than the upwind control region. The mean rainfall rate in the downwind region is 34.4% larger than the upwind region. An analysis of a parameter called the urban rainfall ratio (URR) illustrates that 65% (88%) of the satellite-derived rainfall rates in the downwind (upwind control) region are greater (less) than the mean background rainfall rate of the entire study region. When the data is stratified by summer months from 1998 to 2001 (June-August), even greater influence over and downwind of the urban area is observed in the statistics. This result is consistent with published reports of urban-generated rainfall being more prevalent in the warm season. The research demonstrates that the evolving TRMM satellite climatology is a credible way to detect mesoscale precipitation signatures that may be linked to urbanization. Early results also corroborate recent findings on Houston-induced convection/drainfall anomalies. Burian and Shepherd will report on other aspects of the downscaling analysis in future forums, but early rain gauge results are consistent with the satellite-based observations.

Shepherd, J. Marshall↗
NASA NTRS2003

An Introduction to Atmospheric Radiation: Review for the Bulletin of AMS

Whether you like a certain geophysical book or not, largely depends on your background. The field of radiative transfer and atmospheric radiation, in particular, combines people with a wide range of mathematical skills: from theoretical astrophysicists and nuclear physicists to meteorologists and ecologists. There is always a delicate balance between physical explanations and their mathematical interpretations. This balance is very personal and is based on your background. I came to the field of atmospheric radiative transfer as a mathematician with little knowledge of atmospheric physics. After being in the field for more than a decade, I still have gaps in my atmospheric science education. Thus I assess a radiative transfer book fi-om two main criteria: how well does it describe the material that is familiar to me (the radiative transfer equation and its numerical solutions) and how well does it help me to fill the gaps in my personal knowledge. So I present this review fi-om the perspective of a former mathematician working in the field of atmospheric radiation. . After being asked to review the book, my first intention was to compare the new edition with the previous one (Liou, 1980). In doing so, you can clearly follow the progress made in the field of atmospheric radiation over the past two decades. If there are few changes (as in Fundamental Radiative Transfer) or no changes at all (as in the Maxwell s equations), then the field has not seen much development. To the contrary, many differences between the two editions illustrate areas of major progress in the field, such as evidenced in Thermal Ineared Radiative Transfer and even in the creations of completely new fields like Three-Dimensional Radiative Transfer or Light Scattering by Nonspherical Particles. Obviously, the major changes happened not in the theory, which is at least half a century old, but in data quality and completely new measurements (mostly due to new satellite data) with higher accuracy and more reliability. The new edition illustrates this progress well.

Marshak, Alexander↗
NASA NTRS2006

Mixed Modeling of a SAW Delay Line Using VHDL-AMS

To aid in the development of SAW sensors for aerospace applications we have created a model of a SAW Delay line using VHDL. The model implements the Impulse Response method to calculate the frequency response, impedance, and insertion loss. The model includes optimization for the number of finger pairs in the IDTs and for the aperture height. This paper presents the model and the results from the model for a SAW delay line design.

Wilson, William C.↗
NASA NTRSDate not supplied

Advanced Metal Separation (AMS) via Marangoni Effect-driven Separation

For practical, economical, and sustainable human missions to the Moon, processing of lunar regolith and metal oxides is necessary for localized production of oxygen (O2) and metals that can be repurposed as rocket propellant, life support O2, and in-space manufactured parts. The primary candidates for in-situ resource utilization (ISRU) regolith processing are carbothermic reductions and molten regolith electrolysis (MRE) which both produce oxygen and a reduced, deoxygenated metallic slag. A metal separation technique is still required to capture and purify metals from the deoxygenated slag for reuse in areas such as metallic part fabrication, structural or design frameworks, and metal catalyst production. The Marangoni Effect is best explained as mass transfer along an interface driven by surface tension gradients induced by temperature and concentration differences. Due to the temperature gradients, molten metal can be transported in this fashion to create thin films. This method can transport molten metal in the absence of gravity or mechanical motion and greatly increases the available surface area for a vacuum fractional separation process. In this study, a novel vacuum furnace induces the Marangoni Effect to fractionally decompose and separate valuable metals (e.g., aluminum) from thin films of molten metal via vacuum distillation. The proposed work will examine lunar regolith, metal-based recycling feedstocks, and metallic slags produced from the carbothermal reduction of regolith. Data and observations from this study could produce a simple yet effective method of refining lunar derived metals by taking advantage of the high vacuum environment present on the lunar surface.

ISRU↗
NASA NTRS2007

Risk Assessment of Physiological Effects of Atmospheric Composition and Pressure in Constellation Vehicles

To reduce denitrogenation time to prevent decompression sickness to support frequent extravehicular activities on the Moon, and to limit the risk of fire, a hypobaric (P(sub B) = 414 mmHg) and mildly hypoxic (ppO2 = 132 mmHg, 32% O2 - 68% N2) living environment is being considered during lunar missions for the Crew Exploration Vehicle (CEV) and Lunar Surface Access Module (LSAM). If the vehicular ppO2 is acutely changed from 145-178 mmHg at standard vehicular operating pressure to less than 125 mmHg at desired lunar surface outpost operating pressures, there is the possibility that some crewmembers may develop symptoms of Acute Mountain Sickness (AMS). The signs and symptoms of AMS (headache plus nausea, dizziness, fatigue, or sleeplessness), could impact crew health and performance on lunar surface missions. Methods: An exhaustive literature review on the topic of the physiological effects of reduced ppO2 and absolute pressure as may contribute to the development of hypoxia and altitude symptoms or AMS. The results of the nine most rigorous studies were collated, analyzed and contents on the physiological concerns associated with hypobaric operations, AMS and hypoxia symptoms summarized. Results: Although space vehicles have operated in hypobaric conditions previously, they have not operated in a mildly hypoxic ppO2. There is evidence for an absolute pressure effect per se on AMS, such that the higher the altitude for a given hypoxic alveolar O2 partial pressure (P(sub A)O2), the greater the likelihood of an AMS response. About 25% of adults are likely to experience mild AMS near 2,000 m (xxx mmHg) altitude following a rapid ascent from sea level while breathing air (6,500 feet, acute (P(sub A)O2) = 75 mmHg). The operational experience with the Shuttle staged denitrogenation protocol at 528 mmHg (3,048 m) while breathing 26.5% O2 (acute (P(sub A)O2) = 85 mmHg) in astronauts adapting to microgravity suggests a similar likely experience in the proposed CEV environment. Conclusions: We feel that the slightly elevated risk of AMS with the recommended exploration atmospheric parameters is offset by the DCS risk reduction and improved operational efficiency offered by the hypobaric lunar surface vehicular pressure. We believe the risk of mild AMS is greater given a (P(sub A)O2) of 77 mmHg at 4,876 m altitude while breathing 32% O2 than at 1,828 m altitude while breathing 21% O2. Only susceptible astronauts would develop mild and transient AMS with prolonged exposure to 414 mmHg (4,876 m) while breathing 32% O2 (acute (P(sub A)O2) = 77 mmHg). So the following may be employed for operational risk reduction: 1) develop procedures to increase P(sub B) as needed in the CEV, and use a gradual or staged reduction in cabin pressure during lunar outbound; 2) train crews for symptoms of hypoxia, to allow early recognition and consider pre-adaptation of crews to a hypoxic environment prior to launch, 3) consider prophylactic acetazolamide for acute pressure changes and be prepared to treat any AMS associated symptoms early with both carbonic anhydrase inhibitors and supplemental oxygen.

Scheuring, Richard A.↗
NASA NTRS2007

Risk Assessment of Physiological Effects of Atmospheric Composition and Pressure in Constellation Vehicles

To limit the risk of fire and reduce denitrogenation time to prevent decompression sickness to support frequent extravehicular activities on the Moon, a hypobaric (PB = 414 mmHg) and mildly hypoxic (ppO2 = 132 mmHg, 32% O2 - 68% N2) living environment is considered for the Crew Exploration Vehicle (CEV) and Lunar Surface Access Module (LSAM). With acute change in ppO2 from 145-178 mmHg at standard vehicular operating pressure to less than 125 mmHg at desired lunar surface vehicular operating pressures, there is the possibility that some crewmembers may develop symptoms of Acute Mountain Sickness (AMS). The signs and symptoms of AMS (headache plus nausea, dizziness, fatigue, or sleeplessness), could impact crew health and performance on lunar surface missions. An exhaustive literature review on the topic of the physiological effects of reduced ppO2 and absolute pressure as may contribute to the development of altitude symptoms or AMS was performed. The results of the nine most rigorous studies were collated, analyzed and contents on AMS and hypoxia symptoms summarized. There is evidence for an absolute pressure effect per se on AMS, so the higher the altitude for a given hypoxic alveolar O2 partial pressure (PAO2), the greater the AMS response. About 25% of adults are likely to experience mild AMS near 2,000 m altitude following a rapid ascent from sea level while breathing air (6,500 feet, acute PAO2 = 75 mmHg). The operational experience with the Shuttle staged denitrogenation protocol at 528 mmHg (3,048 m) while breathing 26.5% O2 (acute PAO2 = 85 mmHg) in astronauts adapting to microgravity suggests a similar likely experience in the proposed CEV environment. We believe the risk of mild AMS is greater given a PAO2 of 77 mmHg at 4,876 m altitude while breathing 32% O2 than at 1,828 m altitude while breathing 21% O2. Only susceptible astronauts would develop mild and transient AMS with prolonged exposure to 414 mmHg (4,876 m) while breathing 32% O2 (acute PAO2 = 77 mmHg). So the following may be employed for operational risk reduction: 1) develop procedures to increase PB as needed in the CEV, and use a gradual or staged reduction in cabin pressure during lunar outbound; 2) train crews for symptoms of hypoxia, to allow early recognition and consider pre-adaptation of crews to a hypoxic environment prior to launch, 3) consider prophylactic acetazolamide for acute pressure changes and be prepared to treat any AMS associated symptoms early with both carbonic anhydrase inhibitors and supplemental oxygen.

Scheuring, Richard A.↗
DOE OSTI2025

Changes in atmospheric circulation amplify extreme snowfall fueled by Arctic sea ice loss over high-latitude land

Arctic sea-ice retreat has been linked to increased winter precipitation and heavy snowfall over land, likely due to a combination of enhanced evaporation from ice-free Arctic marginal seas (AMS) and changes in atmospheric circulation. However, their relative roles and contributions remain uncertain. Here, we show that a greater proportion of AMS evaporative moisture reached high-latitude land during the cold seasons from 1980–1989 to 2012–2021. Atmospheric circulation changes added an additional 13 % increase in the AMS moisture contribution, accounting for 11 % of the total increase in AMS-sourced land precipitation. Notably, 46 % of the increase in AMS-sourced extreme snowfall is attributed to circulation-driven landward moisture transport, representing an 84 % increase beyond the effect of enhanced AMS evaporation alone. Further analysis indicates that both the rise in Arctic moisture and the atmospheric circulation shifts are primarily driven by anthropogenic forcing. These findings highlight how atmospheric circulation changes amplify extreme snowfall fueled by AMS evaporation, underscoring the synergistic effects of Arctic sea ice loss and circulation change on high-latitude winter precipitation.

Anthropogenic forcing↗
DOE OSTI2025

National User Resource for Biological Accelerator Mass Spectrometry (Final Report)

The National User Resource for Biological Accelerator Mass Spectrometry (User Resource) will provide isotopic analysis (primarily radiocarbon or 14C) by accelerator mass spectrometry (AMS) for NIH- funded researchers across the United States and will be the only User Resource of its type in the United States. The User Resource will provide measurement capability and expertise to a research community that requires highly sensitive, quantitative isotope analyses. Since commissioning a new accelerator mass spectrometer in June 2014, we have measured over 4000 samples a year for collaborators and service users. The User Resource will enable us to continue to meet these research needs, as well as provide for new users whose research programs would benefit from AMS as a measurement tool. The User Resource’s forte will be ultra-high sensitivity quantitation of radiocarbon and selected other radioisotopes for research studies where isotopes are required. Radioisotope labeling studies have been and will continue to be an important tool for addressing many complex biomedical science problems. AMS is a specialized and unique type of mass spectrometry that provides absolute quantitation of radiocarbon and other relevant radioisotopes with extreme sensitivity, having limits of detection in real samples on the order of a few attomol/mg of sample at measurement precisions of ~3%. It is the only instrumental method capable of quantifying radioisotope-labeled agents routinely in real-world samples with such precision and sensitivity. The sensitivity of AMS allows for the quantification of radiolabeled metabolites in extremely complex matrices of cells and organisms at very low concentrations and in small samples. AMS allows studies to be conducted without perturbing metabolism leading to more relevant quantification of metabolic rates and pathways. In addition, it enables quantification of pharmacokinetic and metabolic properties of toxicants at environmentally relevant concentrations in model systems as well as the ability to quantify pharmacokinetics and other molecular endpoints directly in humans. Such quantitative assessments can 1) improve risk assessment for toxicants, 2) address safety and efficacy considerations for therapeutic entities, 3) deepen understanding of xenobiotic and intermediary metabolism, 4) help understand the interactions between critical molecular pathways, and 5) improve efforts to model and predict various metabolic and biological states. These capabilities have been applied in a number of areas including research in carcinogenesis, toxicology, nutrition, pharmacology/drug development and basic biological science. As a NIGMS National Resource the National User Resource for Biological Accelerator Mass Spectrometry will help NIH funded scientists achieve a deeper understanding of the etiology of human health concerns by (1) enabling the quantification of pharmacokinetics and other molecular endpoints directly in humans; (2) offering the ability to conduct quantitative studies using biologics such as proteins or lipids, and thereby reducing the amount of radioisotope usage in biomedical labs; and (3) enabling more relevant studies of metabolic pathways in health and disease through the use of much lower, more biologically-relevant, concentrations of metabolic substrates in cells and intact organisms. Such studies support NIGMS’s basic biomedical research areas that contribute to the understanding of fundamental cellular and physiological principles and enable research supported by the Biophysics, Biomedical Technology, and Computational Biosciences (BBCB); Genetics and Molecular, Cellular, and Developmental Biology (GMCDB); Pharmacology, Physiology, Biological Chemistry (PPBC) and Training, Workforce Development, and Diversity (TWD) Divisions. Over the next five years, our goals are to: 1. Improve the efficiency of operation for AMS measurements through installation of new interfaces to our AMS systems, technical modifications to improve gas accepting ion source efficiency and upgrading our data analysis software for improved ease of use and data reporting. 2. Increase the accessibility and visibility of ultra-sensitive 14C measurements for the biomedical research community by training of new investigators and expanding our national user base. 3. Provide high throughput, ultra-sensitive 14C analysis for the NIGMS and NIH user community.

47 OTHER INSTRUMENTATION↗
NASA NTRS2002

Speech motor control and acute mountain sickness

BACKGROUND: An objective method that accurately quantifies the severity of Acute Mountain Sickness (AMS) symptoms is needed to enable more reliable evaluation of altitude acclimatization and testing of potentially beneficial interventions. HYPOTHESIS: Changes in human articulation, as quantified by timed variations in acoustic waveforms of specific spoken words (voice onset time; VOT), are correlated with the severity of AMS. METHODS: Fifteen volunteers were exposed to a simulated altitude of 4300 m (446 mm Hg) in a hypobaric chamber for 48 h. Speech motor control was determined from digitally recorded and analyzed timing patterns of 30 different monosyllabic words characterized as voiced and unvoiced, and as labial, alveolar, or velar. The Environmental Symptoms Questionnaire (ESQ) was used to assess AMS. RESULTS: Significant AMS symptoms occurred after 4 h, peaked at 16 h, and returned toward baseline after 48 h. Labial VOTs were shorter after 4 and 39 h of exposure; velar VOTs were altered only after 4 h; and there were no changes in alveolar VOTs. The duration of vowel sounds was increased after 4 h of exposure and returned to normal thereafter. Only 1 of 15 subjects did not increase vowel time after 4 h of exposure. The 39-h labial (p = 0.009) and velar (p = 0.037) voiced-unvoiced timed separations consonants and the symptoms of AMS were significantly correlated. CONCLUSIONS: Two objective measures of speech production were affected by exposure to 4300 m altitude and correlated with AMS severity. Alterations in speech production may represent an objective measure of AMS and central vulnerability to hypoxia.

NASA Discipline Space Human Factors↗
NASA NTRS2011

Asynchronous Message Service Reference Implementation

This software provides a library of middleware functions with a simple application programming interface, enabling implementation of distributed applications in conformance with the CCSDS AMS (Consultative Committee for Space Data Systems Asynchronous Message Service) specification. The AMS service, and its protocols, implement an architectural concept under which the modules of mission systems may be designed as if they were to operate in isolation, each one producing and consuming mission information without explicit awareness of which other modules are currently operating. Communication relationships among such modules are self-configuring; this tends to minimize complexity in the development and operations of modular data systems. A system built on this model is a society of generally autonomous, inter-operating modules that may fluctuate freely over time in response to changing mission objectives, modules functional upgrades, and recovery from individual module failure. The purpose of AMS, then, is to reduce mission cost and risk by providing standard, reusable infrastructure for the exchange of information among data system modules in a manner that is simple to use, highly automated, flexible, robust, scalable, and efficient. The implementation is designed to spawn multiple threads of AMS functionality under the control of an AMS application program. These threads enable all members of an AMS-based, distributed application to discover one another in real time, subscribe to messages on specific topics, and to publish messages on specific topics. The query/reply (client/server) communication model is also supported. Message exchange is optionally subject to encryption (to support confidentiality) and authorization. Fault tolerance measures in the discovery protocol minimize the likelihood of overall application failure due to any single operational error anywhere in the system. The multi-threaded design simplifies processing while enabling application nodes to operate at high speeds; linked lists protected by mutex semaphores and condition variables are used for efficient, inter-thread communication. Applications may use a variety of transport protocols underlying AMS itself, including TCP (Transmission Control Protocol), UDP (User Datagram Protocol), and message queues.

Burleigh, Scott C.↗
NASA NTRS2011

Remote Asynchronous Message Service Gateway

The Remote Asynchronous Message Service (RAMS) gateway is a special-purpose AMS application node that enables exchange of AMS messages between nodes residing in different AMS "continua," notionally in different geographical locations. JPL s implementation of RAMS gateway functionality is integrated with the ION (Interplanetary Overlay Network) implementation of the DTN (Delay-Tolerant Networking) bundle protocol, and with JPL s implementation of AMS itself. RAMS protocol data units are encapsulated in ION bundles and are forwarded to the neighboring RAMS gateways identified in the source gateway s AMS management information base. Each RAMS gateway has interfaces in two communication environments: the AMS message space it serves, and the RAMS network - the grid or tree of mutually aware RAMS gateways - that enables AMS messages produced in one message space to be forwarded to other message spaces of the same venture. Each gateway opens persistent, private RAMS network communication channels to the RAMS gateways of other message spaces for the same venture, in other continua. The interconnected RAMS gateways use these communication channels to forward message petition assertions and cancellations among themselves. Each RAMS gateway subscribes locally to all subjects that are of interest in any of the linked message spaces. On receiving its copy of a message on any of these subjects, the RAMS gateway node uses the RAMS network to forward the message to every other RAMS gateway whose message space contains at least one node that has subscribed to messages on that subject. On receiving a message via the RAMS network from some other RAMS gateway, the RAMS gateway node forwards the message to all subscribers in its own message space.

Wang, Shin-Ywan↗
DOE OSTI2025

Producing 236 U reference standards for Accelerator Mass Spectrometry at the University of Notre Dame

36 U is a rare isotope of uranium, naturally occurring in ores with an abundance of 236 U/ 238 U$<$ 1 x 10 -9 . The ability to detect it and make isotopic ratio measurements has applications ranging from nuclear forensics and nonproliferation to energy production and environmental protection. Currently, Accelerator Mass Spectrometry (AMS) is the only technique sensitive enough to accurately measure 236 U/ 238 U isotopic ratios as they exist in naturally occurring ores in the range of 236 U/ 238 U = 10 -12 $-$ 10 -9 . Some AMS facilities have demonstrated their capabilities to make these measurements. Historically, the lack of commercially available reference standards covering the range of naturally occurring 236 U/ 238 U abundances has necessitated the use of absolute measurements, notoriously difficult to do using AMS, resulting in increased uncertainties in measurements and a reliance on knowledge of systematic effects. To mitigate these issues, various AMS facilities have sought to develop their own reference standards. Using a reference standard prepared for other forms of mass spectrometry, a series of AMS suitable standards was created through dilution with low-background natural uranium. The techniques used to produce and characterize these materials as well as analysis of them using AMS will be discussed.

236U↗
DOE OSTI2024

Exploring the potential and impact of single-crystal active materials on dry-processed electrodes for high-performance lithium-ion batteries

Roll-to-roll powder-to-film dry processing (DP) and single-crystal (SC) active materials (AMs) with many advantages are two hot topics of lithium-ion batteries (LIBs). However, DP of SC AMs for LIBs is rarely reported. Consequently, the impact of SC AMs on dry-processed LIBs is not well understood. Herein, for the first time, via a set of experimental and theoretical studies of the conventional polycrystalline-AM- and SC-AM-based DPed electrodes (DPEs), this work not only reports a high-performance dry SC-AM cathode for LIB manufacturing, but also establishes some fundamental understanding of SC-based dry-processed electrodes, including their morphology, structure, mechanical strength, electronic conductivity and LIB electrochemical behavior. Further, the results suggest that DP of SC AMs is promising, which can dramatically improve the electrochemical kinetics at electrode level and particle level. Specifically, for the rate capability and long-term cyclability in full cells, SC DPEs exhibit a discharge specific capacity of 152.1 mAh g -1 at 1C and a capacity retention rate of 79.9 % at C/3 over 500 cycles, which are superior to those of PC DPEs (135.6 mAh g -1 and 68.3 %) at the same conditions and are further confirmed by the simulation data from the theoretical modelling study. Therefore, this comprehensive work marks a significant milestone for DP strategy and SC AMs, enlightening future research and development of LIB manufacturing.

25 ENERGY STORAGE↗
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↗
DOE OSTI2024

Technical note: Optimizing the in situ cosmogenic 36 Cl extraction and measurement workflow for geologic applications

Abstract. In situ cosmogenic 36Cl analysis by accelerator mass spectrometry (AMS) is routinely employed to date Quaternary surfaces and assess rates of landscape evolution. However, standard laboratory preparation procedures for 36Cl dating require the addition of large amounts of isotopically enriched chlorine spike solution; these solutions are expensive and increasingly difficult to acquire from commercial sources. In addition, the typical workflow for 36Cl dating involves measuring both 35Cl/37Cl and 36Cl/Cl concurrently on the high-energy (post-accelerator) end of the AMS system, but 35Cl/37Cl determinations using this technique can be complicated by isotope fractionation and system memory during measurement. The traditional workflow also does not provide 36Cl extraction laboratories with the data needed to calculate native Cl concentrations in advance of 36Cl/Cl measurements. In light of these concerns, we present an improved workflow for extracting and measuring chlorine in geologic materials. Our initial step is to characterize 35Cl/37Cl on sample aliquots of up to ∼1 g prepared in Ag(Cl, Br) matrices, which greatly reduces the amount of isotopically enriched spike solution required to measure native Cl content in each sample. To avoid potential issues with isotope fractionation through the accelerator, 35Cl/37Cl is measured on the low-energy, pre-accelerator end of the AMS line. Then, for 36Cl/Cl measurements, we extract Cl as AgCl or Ag(Cl, Br) in analytical batches with a consistent total Cl load across all samples; this step is intended to minimize source memory effects during 36Cl/Cl measurements and allows the preparation of AMS standards that are customized to match known Cl contents in the samples. To assess the efficacy of this extraction and measurement workflow, we compare chlorine isotope ratio measurements on seven geologic samples prepared using standard procedures and the updated workflow. Measurements of 35Cl/37Cl and 36Cl/Cl are consistent between the two workflows, and 35Cl/37Cl values measured using our methods have considerably higher precision than those measured following standard protocols. The chemical preparation and measurement workflow presented here (1) reduces the amount of isotopically enriched chlorine spike used per rock sample by up to 95 %; (2) identifies rocks with high native Cl concentrations, which may be lower priority for 36Cl surface exposure dating, at an early stage of analysis; and (3) allows laboratory users to maintain control over the total chlorine content within and across analytical batches. These methods can be incorporated into existing laboratory and AMS protocols for 36Cl analyses and will increase the accessibility of 36Cl dating for geologic applications.

58 GEOSCIENCES↗