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NASA NTRS2007

Strain Measurement Using FBG on COPV in Stress Rupture Test

White Sands Test Facility (WSTF) was requested to perform ambient temperature hydrostatic pressurization testing of a Space Transportation System (STS) 40-in. Kevlar Composite Overwrapped Pressure Vessel (COPV). The 40-in. vessel was of the same design and approximate age as the STS Main Propulsion System (MPS) and Orbiter Maneuvering System (OMS) vessels. The NASA Engineering Safety Center (NESC) assembled a team of experts and conducted an assessment that involved a review of national Kevlar COPY data. During the review, the STS COPVs were found to be beyond their original certification of ten years. The team observed that the likelihood of STS COPV Stress rupture, a catastrophic burst before leak failure mode, was greater than previously believed. Consequently, a detailed assessment of remaining stress rupture life became necessary. Prior to STS-114, a certification deviation was written for two flights of OV-103 (Discovery) and OV-104 (Atlantis) per rationale that was based on an extensive review of the Lawrence Livermore National Laboratories, COPV data, and revisions to the STS COPV stress levels. In order to obtain flight rationale to extend the certification deviation through the end of the Program, the Orbiter Project Office has directed an interagency COPV team to conduct further testing and analysis to investigate conservatism in the stress rupture model and evaluate material age degradation. Additional analysis of stress rupture life requires understanding the fiber stresses including stress that occurs due to thru-wall composite compression in COPV components. Data must be obtained at both zero gauge pressure (pre-stress) and at the component operating pressure so that this phenomenon can be properly evaluated. The zero gauge pressure stresses are predominantly a result of the autofrettage process used during vessel manufacture. Determining these pre-stresses and the constitutive behavior of the overwrap at pressure will provide necessary information to better predict the remaining life of the STS COPVs. The primary test objective is obtaining data to verify the hypothesis of a radially oriented thru-thickness stress-riser in the COPV composite whose magnitude is a function of the applied pressure and the load history. The anticipated load dependent response follows from the constitutive behavior of the composite overwrap so data to quantify its nonlinear and time dependent response will be sought. The objective of the Fiber Braggs Gratings (FBGs) were to advance the state-of-the-art by developing techniques using FBG sensors that are capable of assessing stress-rupture degradation in Kevlar COPVs in a health monitoring mode (1). Moreover, they sought to answer questions of how embedded sensors affect overall integrity of the structure. And lastly, they sought to provide an important link in the overall stress rupture study that will help close the loop on the COPV fabrication process. NDE inspection methods will be used from start to finish and FBG will be an integral link within the overall chain.

Banks, Curtis↗

DOE OSTI2022

Precursor Analysis Report: Industroyer Targeting Ukraine Electric Power Transport Utility (Ukrenergo) 2016

The Industroyer Targeting Ukraine Electric Power Transport Utility (Ukrenergo) 2016 Precursor Analysis Report leverages publicly available information about the December 2016 cyber attack against the Ukrainian Ukrenergo electric transmission utility and catalogs anomalous observables for each technique employed in the attack. This analysis is based upon the methodology of the Cybersecurity for the Operational Technology Environment (CyOTE) program. Industroyer is a modular malware framework designed to deploy several Industrial Control System (ICS) protocol-specific attack payloads to disrupt electricity distribution. Adversaries deployed Industroyer within the target network on a Microsoft Windows endpoint capable of directly manipulating or communicating with ICS. Industroyer abuses the functionality of a targeted ICS’s legitimate control system to achieve its intended impact. Adversaries likely first gained access to Ukrenergo enterprise networks in early 2016 after a successful spearphishing campaign against organizations in the electric power sector. Adversaries then began capturing credentials beginning on 1 December 2016. This allowed access to the ICS environment at the Pivnichna electric transmission substation outside Kyiv through a device dual-homed on the Information Technology (IT) and ICS networks. Adversaries conducted discovery, targeting, and access to this device using information and previously captured credentials from compromised enterprise IT machines. Finally, the adversaries deployed and launched the Industroyer malware just before midnight on 17 December. By midnight, Ukrenergo had lost control of a targeted substation, resulting in electric power outages for over an hour in the city of Kyiv and the Kyiv region. Researchers and analysts identified 31 unique techniques (used in a sequence of 33 steps) utilized during the attack with a total of 846 observables using MITRE ATT&CK® for Industrial Control Systems. The CyOTE program assesses observables accompanying techniques used prior to the triggering event to identify opportunities to detect malicious activity. If observables accompanying the attack techniques are perceived and investigated prior to the triggering event, earlier comprehension of malicious activity can take place. Twenty-nine of the identified techniques used during the Industroyer cyber attack were precursors to the triggering event. Analysis identified 548 observables associated with these precursor techniques, 353 of which were assessed to have an increased likelihood of being perceived in the 300 days preceding the triggering event. The response and comprehension time could have been reduced if the observables had been identified earlier. The information gathered in this report contributes to a library of observables tied to a repository of artifacts, data sources, and technique detection references for practitioners and developers to support the comprehension of indicators of attack. Asset owners and operators can use these products if they experience similar observables or to prepare for comparable scenarios.

45 MILITARY TECHNOLOGY, WEAPONRY, AND NATIONAL DEF↗

NASA NTRSDate not supplied

Neo – Mars Adaptive Training Integrative Knowledge System (MATRIKS) to Improve Operational Performance and its Neural Basis for Spaceflight

With prolonged mission durations, spaceflight crews will become increasingly dependent on onboard technologies for knowledge acquisition and maintenance. It is expected that not all skills and knowledge required for these missions can be retained and retrieved based on pre-mission training alone. Limited and delayed communication will significantly constrain support from Mission Control and crews will increasingly rely on autonomous onboard technologies to successfully perform post-landing operations. With the present project we will target NASA’s particular interest in developing and assessing an adaptive, just-in-time countermeasure that will consolidate and improve skills that are most relevant to space flight operations. To achieve this aim, NASA established a Virtual NASA Specialized Center of Research (VNSCOR)referred to as “Mars Adaptive Training Integrative Knowledge System (MATRIKS)”, comprising the following three projects: (1) “Trinity–Multi-Environment Virtual Training for Long Duration Exploration Missions”, PI: A. Anderson (UC Boulder); (2) “Morpheus–A Haptic Sensory Supplement to Optimize In-Flight Adaptive Training for Human Control of Spacecraft Robotic Arms”, PI: S. Robinson, UC Davis); and the present project “Neo–Adaptive Training integrative knowledge System to Improve Operational Performance and its Neural Basis for Spaceflight” (UPenn, PI: A.C. Stahn). Neo leverages a validated workstation called 6DF that simulates a rendezvous and docking maneuver using real spacecraft flight dynamics. It is designed to (1) train and improve sensorimotor skills relevant for inflight and post-landing operational tasks; (2) feature an autonomous and adaptive training approach that does not rely on feedback from flight operations on the ground; (3) maximize the transfer of mission-relevant motor skills; (4) allow the assessment of the neural circuitry underlying the task; and (5) deliver the training in a motivating and meaningful way to astronauts. Neocomprises two overarching aims: First, we will identify the neural circuitry underlying spaceflight relevant tasks by performing a subset of the 6DFtaskduring functional magnetic resonance imaging (MRI)in a total of up to N=30 subjects with varying levels of 6DF training experience. Second, as part of the above-mentioned VNSCOR MATRIKS the proposed 6DF autonomous intelligent tutor system will be integrated in an additive manner with a haptic feedback intervention (Morpheus), and a multi-environment virtual trainer(Trinity).It is expected that Neo, Morpheus and Trinity mutually complement each other to facilitate an effective countermeasure tool to acquire and retain operational skills that are critical for exploration class missions. To assess the efficacy of this combined effort, the VNSCOR MATRIKS will collect data inN=16 crew members in one HERA campaign of 45 days duration with N=16 crew members(four missions with N=4 crew member seach).The primary goal is to identify changes in operational performance as assessed by NASA’s simulator of Canadarm2 operations, i.e., Robotic On-board Trainer (ROBoT-r) in response to MATRIKS. As part of Neo we will also identify if, and to what extent MATRIKS will promote transfer to general cognitive performance (Cognition battery), distinctive visuo-spatial tasks critical for telerobotic tasks (Spatial Cognition battery), and affect brain structural changes and the neural circuitry of key brain networks expected to be relevant for spaceflight-related performance. At the conclusion of the research, we will have defined and demonstrated the use of a neuroscience-based, adaptive training integrative knowledge system to potentially mitigate visuo-spatial and sensorimotor brain changes associated with prolonged isolation and confinement to reduce the likelihood or impact of potential decrements in human performance capabilities during long-duration space missions. The expected significance of this 4-year project relates to its relevance for facilitating effective countermeasure tools to acquire and retain operational skills that are critical for exploration class missions. This will support the development of necessary countermeasures and technologies in support of human space exploration, focusing on mitigating operational performance risks.

A C Stahn↗

NASA NTRS1996

Early Energetic Particle Irradiation of the HED Parent Body Regolith

Previous studies have shown that many individual grains within the dark phase of the Kapoeta howardite were irradiated with energetic particles while residing on the surface of the early HED regolith. Particle tracks in these grains vary in density by more than an order of magnitude and undoubtedly were formed by energetic heavy (Fe) ions associated with early solar flares. Early Irradiation of HED Regolith: Concentrations of excess Ne alone are not sufficient to decide between competing galactic and solar irradiation models. However, from recent studies of depth samples of oriented lunar rocks, we have shown that the cosmogenic 21-Ne/22-Ne ratio produced in feldspar differs substantially between Galactic Cosmic Radiation (GCR) and solar protons, and that this difference is exactly that predicted from cross-section data. Using Ne literature data and new isotopic data we obtained on acid-etched, separated feldspar from both the light and dark phases of Kapoeta, we derive 21-Ne/22-Ne = 0.80 for the recent GCR irradiation and 21-Ne/22-Ne = 0.68 for the early regolith irradiation. This derived ratio indicates that the early Ne production in the regolith occurred by both galactic and solar protons. If we adopt a likely one-component regolith model in which all grains were exposed to galactic protons but individual grains had variable exposure to solar protons, we estimate that this early GCR irradiation lasted for about 3-6 m.y. More complex two-component regolith models involving separate solar and galactic irradiation would permit this GCR age to be longer. Higher-energy solar protons would permit the GCR to be longer. Higher-energy solar protons would permit the GCR age to be shorter. Further, cosmogenic 126(Xe) in Kapoeta dark is no more than a factor of about 2 higher than that observed in Kapoeta light. Because 126(Xe) can only be formed by galactic protons and not solar protons, these data support a short GCR irradiation for the HED regolith. This would also be the maximum time peRiod for the solar irradiation. Various asteroidal regolith models, based on Monte Carlo modeling of impact rates as a function of size and on irradiation features of meteorites, predict surface exposure times of about 0.1 to 10 m.y., and depend on such factors as gravity, rock mechanical properties, and micrometeoroid flux. Because the depth at which solar Fe tracks are produced (is much less than 1 micrometer) is much less than the depth at which Solar Cosmic Rays (SCR) Ne is produced (about 1 cm), for a reasonably well-stirred HED regolith the "surface exposure time" for SCR 21-Ne production should be significantly longer than that for solar tracks and some other surface irradiation features. Enhanced Solar Proton Irradiation: For bulk samples of Kapoeta dark feldspar and a one-component regolith model, the derived ratio of 21-Ne/22-Ne = 0.68 implies that the early production ratio of SCR 21-Ne to GCR 21-Ne was about 0.5-1.5. This ratio is independent of any assumptions about the fraction of dark grains that are irradiated or of the variability in the degree of solar irradiation among grains. The 21-Ne SCR/GCR ratio indirectly derived from bulk Kapoeta pyroxene is somewhat larger, as is the ratio derived for simple two-component regolith models. Individual feldspar grains that were extensively solar irradiated would require even larger 21-Ne SCR/GCR production ratios. In contrast, the theoretical SCR/GCR production ratio for lunar feldspar with 0 g/CM2 shield ing is is less than or equal to 2, and the lowest ratio observed in near-surface samples of lunar anorthosites is less than or equal to 1. Considering the greater solar distance of Vesta (compared to the Moon), the likelihood that SCR 21-Ne was acquired under some shielding where production rates are lower, and the likelihood that the exposure time to galactic protons exceeded the exposure time to solar protons because of their very different penetration depths, the 21-Ne SCR/GCR production ratio on the HED parent body was probably < 0.1. The relatively large difference between the derived 21-Ne SCR/GCR ratio in Kapoeta dark feldspar and the estimated production ratio strongly indicates that the early solar irradiation involved a flux -20-50x the recent solar flux. This enhanced proton flux was probably associated with an overall greater solar activity in the first approximately 10(exp 7) to 10(exp 8) years of solar history.

Bogard, D. D.↗

DOE OSTI2022

Precursor Analysis Report: Conti Ransomware Attack on the Health Service Executive of Ireland 2021

The Conti Ransomware Attack on the Health Service Executive (HSE) of Ireland 2021 Precursor Analysis Report leverages publicly available information about the attack and catalogs anomalous observables for each technique employed by the adversary. This analysis is based upon the methodology of the Cybersecurity for the Operational Technology Environment (CyOTE) program. The HSE provides public healthcare corporate services and operational services throughout Ireland, with critical functions including the acute national ambulance service, acute hospital service, and community healthcare service. On 14 May 2021, Conti ransomware encrypted 80 percent of the HSE’s Information Technology (IT) infrastructure across corporate, hospital, community, and electronic health record services. Conti is a ransomware-as-a-service operation that encrypts local files, uses double extortion against victims, and is facilitated by many intrusion tools. The attack forced the HSE to shut down its entire IT infrastructure to contain the ransomware, forcing employees to revert to pen and paper recordkeeping and leading to the cancellation of many appointments and procedures. The adversary also exfiltrated 700 GB of data, compromising the confidentiality of patients’ protected health information. Had the adversary targeted the COVID-19 cloud systems or operational technology assets, such as Internet of Medical Things medical devices or smart building management systems, the impact of the attack would almost certainly have been far more severe. Researchers and analysts identified 21 unique techniques (used in a sequence of 23 steps) likely utilized during the attack with a total of 1,185 observables using MITRE ATT&CK® for Industrial Control Systems. The CyOTE program assesses observables accompanying techniques used prior to the triggering event to identify opportunities to detect malicious activity. If observables accompanying the attack techniques are perceived and investigated prior to the triggering event, earlier comprehension of malicious activity can take place. Twenty-one of the identified techniques used during the attack on the HSE were precursors to the triggering event. Analysis identified 1,086 observables associated with these precursor techniques, 850 of which were assessed to have an increased likelihood of being perceived in the 57 days preceding the triggering event. The response and comprehension time could have been reduced if the observables had been identified earlier. The information gathered in this report contributes to a library of observables tied to a repository of artifacts, data sources, and technique detection references for practitioners and developers to support the comprehension of indicators of attack. Asset owners and operators can use these products if they experience similar observables or to prepare for comparable scenarios.

45 MILITARY TECHNOLOGY, WEAPONRY, AND NATIONAL DEF↗

NASA NTRS1996

Uncertainty and Intelligence in Computational Stochastic Mechanics

Classical structural reliability assessment techniques are based on precise and crisp (sharp) definitions of failure and non-failure (survival) of a structure in meeting a set of strength, function and serviceability criteria. These definitions are provided in the form of performance functions and limit state equations. Thus, the criteria provide a dichotomous definition of what real physical situations represent, in the form of abrupt change from structural survival to failure. However, based on observing the failure and survival of real structures according to the serviceability and strength criteria, the transition from a survival state to a failure state and from serviceability criteria to strength criteria are continuous and gradual rather than crisp and abrupt. That is, an entire spectrum of damage or failure levels (grades) is observed during the transition to total collapse. In the process, serviceability criteria are gradually violated with monotonically increasing level of violation, and progressively lead into the strength criteria violation. Classical structural reliability methods correctly and adequately include the ambiguity sources of uncertainty (physical randomness, statistical and modeling uncertainty) by varying amounts. However, they are unable to adequately incorporate the presence of a damage spectrum, and do not consider in their mathematical framework any sources of uncertainty of the vagueness type. Vagueness can be attributed to sources of fuzziness, unclearness, indistinctiveness, sharplessness and grayness; whereas ambiguity can be attributed to nonspecificity, one-to-many relations, variety, generality, diversity and divergence. Using the nomenclature of structural reliability, vagueness and ambiguity can be accounted for in the form of realistic delineation of structural damage based on subjective judgment of engineers. For situations that require decisions under uncertainty with cost/benefit objectives, the risk of failure should depend on the underlying level of damage and the uncertainties associated with its definition. A mathematical model for structural reliability assessment that includes both ambiguity and vagueness types of uncertainty was suggested to result in the likelihood of failure over a damage spectrum. The resulting structural reliability estimates properly represent the continuous transition from serviceability to strength limit states over the ultimate time exposure of the structure. In this section, a structural reliability assessment method based on a fuzzy definition of failure is suggested to meet these practical needs. A failure definition can be developed to indicate the relationship between failure level and structural response. In this fuzzy model, a subjective index is introduced to represent all levels of damage (or failure). This index can be interpreted as either a measure of failure level or a measure of a degree of belief in the occurrence of some performance condition (e.g., failure). The index allows expressing the transition state between complete survival and complete failure for some structural response based on subjective evaluation and judgment.

Ayyub, Bilal M.↗

NASA NTRS2015

Integrated Medical Model Project - Overview and Summary of Historical Application

Introduction: The Integrated Medical Model (IMM) Project represents one aspect of NASA's Human Research Program (HRP) to quantitatively assess medical risks to astronauts for existing operational missions as well as missions associated with future exploration and commercial space flight ventures. The IMM takes a probabilistic approach to assessing the likelihood and specific outcomes of one hundred medical conditions within the envelope of accepted space flight standards of care over a selectable range of mission capabilities. A specially developed Integrated Medical Evidence Database (iMED) maintains evidence-based, organizational knowledge across a variety of data sources. Since becoming operational in 2011, version 3.0 of the IMM, the supporting iMED, and the expertise of the IMM project team have contributed to a wide range of decision and informational processes for the space medical and human research community. This presentation provides an overview of the IMM conceptual architecture and range of application through examples of actual space flight community questions posed to the IMM project. Methods: Figure 1 [see document] illustrates the IMM modeling system and scenario process. As illustrated, the IMM computational architecture is based on Probabilistic Risk Assessment techniques. Nineteen assumptions and limitations define the IMM application domain. Scenario definitions include crew medical attributes and mission specific details. The IMM forecasts probabilities of loss of crew life (LOCL), evacuation (EVAC), quality time lost during the mission, number of medical resources utilized and the number and type of medical events by combining scenario information with in-flight, analog, and terrestrial medical information stored in the iMED. In addition, the metrics provide the integrated information necessary to estimate optimized in-flight medical kit contents under constraints of mass and volume or acceptable level of mission risk. Results and Conclusions: Historically, IMM simulations support Science and Technology planning, Exploration mission planning, and ISS program operations by supplying simulation support, iMED data information, and subject matter expertise to Crew Health and Safety and the HRP. Upcoming release of IMM version 4.0 seeks to provide enhanced functionality to increase the quality of risk decisions made using the IMM through a more accurate representation of the real world system.

Myers, J.↗

NASA NTRS2024

Evaluating Liftoff Debris for NASA’s Space Launch System (SLS) Prior to the Artemis I Launch

The SLS Artemis I launch vehicle is the first of several planned Artemis launch vehicles, with a number of design differences from earlier NASA missions that incur liftoff debris risk to the mission. As a test vehicle, the Artemis I hardware also endured environments and tests not planned for future missions, which led to several additional factors contributing to an evolving liftoff debris risk to the SLS vehicle. This paper will summarize these risk factors and address the processes used to evaluate and communicate the risks to support a successful Artemis I launch. It will discuss how the evolving risks that were quantified and evaluated by a Cross-Program team of debris Subject Matter Experts to mitigate liftoff debris hazards and communicate updated risk to the SLS vehicle. This process was performed through the inaugural use of an SLS debris day-of-launch (DOL) standard operating procedure that will be used for subsequent Artemis missions. This paper addresses the risk of liftoff debris, debris released by the vehicle or from the launch pad during liftoff through vehicle tower clear. Expected liftoff debris is well understood from previous NASA programs’ experience and from tests of materials, processes and functions that are known to release liftoff debris. These expected sources were assessed and cleared well ahead of launch day. However, given the ever-changing schedules and environments, processes were in place to evaluate any additional potential liftoff debris risks identified during launch countdown. Although many of the Artemis vehicle hardware components are similar to those on the NASA Shuttle Program, there are important differences in the architecture of the Artemis I vehicle which require new assessments of liftoff debris risk for the Artemis missions. The more favorable Artemis crew module location and surfaces are far less vulnerable to debris impacts; however, the longer vehicle can result in higher liftoff debris impact energies to those components on the aft end of the vehicle. Additionally, the positional change of the RS-25 liquid engines to nearer the Booster nozzle exit plane along with the change in Booster throat plug design is a disadvantage to the overall liftoff debris risk which resulted in additional test and analysis efforts for evaluating the integrated vehicle debris risk. In spite of the comprehensive tests and analyses of Artemis I expected liftoff debris, a number of additional tests/processes were completed prior to the Artemis I mission that were required to support a complete understanding of a new launch vehicle, but increased the risk of releasing liftoff debris. The hardware endured several additional cryogenic loading cycles, including the Green Run tests at Stennis Space Center, Wet Dress Rehearsals at Kennedy Space Center, and multiple launch attempts. Each of these cycles induced stresses in the thermal protection system (TPS) materials, increasing the risk of damage to and release of the TPS. Additionally, induced and weather environmental factors that could increase the likelihood of debris release were significant. Vibrations and stresses in the TPS were induced by a required roll-back to the Vehicle Assembly Building before Hurricane Ian to protect the vehicle from damage by high winds. Wind damage and potential internal stresses to several outer mold line materials on the integrated SLS vehicle and mobile launcher were caused by weathering Hurricane Nicole at Pad 39B the week before launch. A thorough imagery scan of the vehicle was performed after each event and the damage observed was repaired, removed, or assessed and the risk to the mission evaluated. Mitigation of debris risk can occur by tests and analyses to show debris impacted components as damage tolerant, by new/improved processes for prevention of debris availability, or redesign. Risk mitigation processes for Artemis I-specific liftoff debris events and the development and use of the SLS debris day of launch (DOL) procedures that will be used for subsequent Artemis missions will be described.

Space Launch System↗

NASA NTRSDate not supplied

Evaluating Liftoff Debris for NASA’s Space Launch System (SLS) Prior to the Artemis I Launch

Space Launch System↗

NASA NTRS1962

Titanium-Oxygen Reactivity Study

A program has been conducted at Astronautics to investigate the likelihood of occurrence of the catastrophic oxidation of titanium alloy sheet under conditions which simulate certain cases of accidental failure of the metal while it is in contact with liquid or gaseous oxygen. Three methods of fracturing the metal were used; they consisted of mechanical puncture, tensile fracture of welded joints, and perforation by very high velocity particles. The results of the tests which have been conducted provide further evidence of the reactivity of titanium with liquid and gaseous oxygen. The evidence indicates that the rapid fracturing of titanium sheet while it is in contact with oxygen initiates the catastrophic oxidation reaction. Initiation occurred when the speed of the fracture was some few feet per second, as in both the drop-weight puncture tests and the static tensile fracture tests of welded joints, as well as when the speed was several thousand feet per second, as in the simulated micrometeoroid penetration tests. The slow propagation of a crack, however, did not initiate the reaction. It may logically be concluded that the localized frictional heat of rapid fracture and/or spontaneous oxidation (exothermic) of minute particles emanating from the fracture cause initiation of the reaction. Under conditions of slow fracture, however, the small heat generated may be adequately dissipated and the reaction is not initiated. A portion of the study conducted consisted of investigating various means by which the reaction might be retarded or prevented. Providing a "barrier" at the titanium-oxygen interface consisting of either aluminum metal or a coating of a petroleum base corrosion inhibitor appeared to be only partially effective in retarding the reaction. The accidental puncturing or similar rupturing of thin-walled pressurized oxygen tanks on missiles and space vehicle will usually constitute loss of function, and may sometimes cause their catastrophic destruction by explosive decompression regardless of the type of material used for their construction. In the case of tanks constructed of titanium alloys the added risk is incurred of catastrophic burning of the tanks. In view of this it is recommended that thin-walled tanks constructed of titanium alloys should not be used to contain liquid or gaseous oxygen.

Chafey, J. E.↗

DOE OSTI2022

Novel Amorphous Carbons for the Adsorption of Phosphate: Part I. Elucidation of Chemical Structure of N-Metal-Doped Chars

Due to phosphate’s necessity in agriculture and its danger to the environment, the development of adsorbents for its removal has been the subject of intensive research activity. Although the introduction of nitrogen functionality to chars and modification of biochar with metals have proven to change the character of the char structure, making it more active toward nutrients, there is no study regarding the doping of biochar with metals and nitrogen simultaneously for the adsorption of phosphates. This paper is the first of two in which we report the production, characterization, and evaluation of N-metal-doped biochars from cellulose for phosphate removal from liquid effluents. In this part, we describe the production and characterization of N-Ca-, N-Fe-, and N-Mg-doped biochars. The elemental composition and surface area of each of the materials produced is reported. Elemental and surface characterization of the chars are reported with the largest N content appearing at a temperature of 800 °C (12.5 wt %) and a maximum surface area for biochar produced at 900 °C (1314 m2/g). All of the adsorbents were visualized by scanning electron microscope (SEM), confirming that although there are some crystals on the surface of the biochar produced, most of the N, Mg, and Ca are part of the polyaromatic ring structure. Transmission electron microscope (TEM) images clearly show the formation of nanoclusters with the metals in the case of N-Fe and N-Ca biochars. The N-Mg biochars show a uniform distribution of the Mg through the carbon surface. X-ray photoelectron spectroscopy (XPS) studies of the biochars produced with metals and varying nitrogen levels clearly show Mg and Ca peaks shifting their position in the presence of N, suggesting the formation of stable structures between metals and N in the carbon polyaromatic ring system. To elucidate the nature of these structures, we conducted DFT-based calculations on different configurations of the nitrogenated structures. The calculated binding energy shifts were found to closely match the XPS experimental binding energy, confirming the likelihood of these structures in biochar. Finally, based on our experimental and modeling results, we hypothesize that an important fraction of the Mg and Ca is introduced to these biochars at the edges. Another fraction of Mg and Ca is in the form of phthalocyanine-like internal structures. More experimental studies are needed to confirm the formation of these very interesting structures and their potential use as adsorbents or catalysts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2016

Low Temperature Regolith Bricks for In-Situ Structural Material

Current technology for producing in-situ structural materials on future missions to Mars or the moon relies heavily on energy-intensive sintering processes to produce solid bricks from regolith. This process requires heating the material up to temperatures in excess of 1000 C and results in solid regolith pieces with compressive strengths in the range of 14000 to 28000 psi, but are heavily dependent on the porosity of the final material and are brittle. This method is currently preferred over a low temperature cementation process to prevent consumption of precious water and other non-renewable materials. A high strength structural material with low energy requirements is still needed for future colonization of other planets. To fulfill these requirements, a nano-functionalization process has been developed to produce structural bricks from regolith simulant and shows promising mechanical strength results. Functionalization of granular silicate particles into alkoxides using a simple low temperature chemical process produces a high surface area zeolite particles that are held together via inter-particle oxygen bonding. Addition of water in the resulting zeolite particles produces a sol-gel reaction called "inorganic polymerization" which gives a strong solid material after a curing process at 60 C. The aqueous solution by-product of the reaction is currently being investigated for its reusability; an essential component of any ISRU technology. For this study, two batches of regolith bricks are synthesized from JSC-1A; the first batch from fresh solvents and chemicals, the second batch made from the water solution by-product of the first batch. This is done to determine the feasibility of recycling necessary components of the synthesis process, mainly water. Characterization including BET surface area, SEM, and EDS has been done on the regolith bricks as well as the constituent particles,. The specific surface area of 17.53 sq m/g (average) of the granular regolith material was obtained from nitrogen adsorption isotherm measurement. The size, shape and textures of regolith from SEM shows that the particles are 25-50 micrometers in size and mostly irregular in shape (Figure 1a). The elemental composition of regolith was identified from EDS analysis showed the presence of Si, Al, Fe, Na, Mg, Ca, Ti, O and C (see figure 1b). Each set of cylindrical brick samples were prepared by low energy process, and cured for 21 and 28 days, respectively to compare their compressive strength. Figure 1c, and d shows the JSC-1A brick and the compressive strength measurements. The results from the 21 day cured bricks (2 bricks) have been done and yielded an aver-age strength of 3050 psi, considerably higher than Portland cement mortars (Type IV and V). This promising technology provides the benefits of construction material similar to concrete, with a low complexity, low energy synthesis process and the likelihood of complete reusability of precious resources. Compressive strength using this method can be improved by increasing the surface area of the particles, using bi-modal particle size distribution, and adding certain additives to increase inter-particle forces.

ISRU↗

NASA NTRSDate not supplied

The Effect of Temperature on the Preservation of Volatile-Rich Lunar Samples

Introduction. The Moon’s south pole is a high-priority target for human exploration and scientific study. This interest is, in part, due to the presence of Permanently Shadowed Regions (PSRs), which could contain high concentrations of unique volatiles at cryogenic temperatures [1]. Returned samples from PSRs may include a unique combination of rocks, regolith, and volatile species, providing unprecedented insights into the history of the Solar System and the potential for resource utilization on the Moon. However, because PSR samples are cryogenic up-on collection, lunar polar sample return will eventually require cold stowage for the journey from the Moon to Earth. Without cold stowage, PSR sample return will likely result in phase changes and chemical reactions within the volatile component of the sample, which would negatively impact the resulting scientific studies of those samples. This abstract summarizes the initial results from an ongoing characterization of analog PSR samples at a range of temperatures, with the goal of defining the temperatures needed for a flight cold stowage freezer. Background. Based on remote sensing observations of the Moon [2], south polar PSRs range in temperature from ~120K for small and/or shallow PSRs to ~20K at the most extreme locations in large, deep PSRs. A range of volatiles have been hypothesized to exist at the surface or subsurface of the lunar poles [3-5 and others]. This hypothesis was verified when the LCROSS mission impacted the <50-K PSR in the crater Cabeus, detecting a range of volatiles from water to low condensation temperature species such as H2S and methane [6]. Species such as H2S and ammonia (also detected by LCROSS) are also highly reactive, and increase the likelihood of chemical reactions at elevated (non-cryogenic) temperatures. At the Johnson Space Center’s Planetary Exploration and Astromaterials Research Laboratory (JSC-PEARL), we have developed a volatile-bearing lunar simulant that incorporates several of the species detected by LCROSS [Table 1] mixed cryogenically with the USGS Lunar Highlands Type (LHT) regolith simulant. The new volatile-regolith simulant will be used to assess the degree of sample alteration at room temperature, -20°C, -80°C, and -196°C (liquid nitro-gen), over a two-week period. Room temperature samples represent those likely to be returned during initial missions without cold stowage, -20°C provides an analog to Apollo cold curated samples, -80°C is the temperature of multiple flight payload freezers (e.g., MELFI), and -196°C is analogous to lunar PSRs. Two weeks is an approximation of the time between sample collection and Earth return for initial Artemis missions. Over this period of time, sample head-space gases will be analyzed using a Universal Gas Analyzer (UGA, a type of mass spectrometer) coupled with a Baratron pressure sensor. After testing, the regolith component of the simulant will be purged of volatiles and preserved for future electron beam and/or FTIR analysis. Experimental Procedure. Volatile-regolith simulants will be produced as an initial homogenous batch; this batch will then be distributed into aliquots (gas chromatography/GC vials or cryo vials), ensuring that each sample has the same starting composition and conditions [Fig. 1]. In addition to the “full” simulant shown in Table 1, less complex simulant compositions will be used as baseline and control samples [Table 2]. Aliquots will be produced in triplicate for each simulant composition, storage temperature, and date of sampling. Headspace gases in all Day 0 samples will be analyzed by the UGA immediately. Cold storage samples for future analytical days will be placed in freezers appropriate to their target temperatures (-20°C, -80°C, -196°C). For ambient-temperature samples, regolith and regolith-water samples will be stored in a fume hood, while the full simulant will be stored in a sealed Parr vessel for safety; no other simulants (RWCM/ RWCM+) will be stored at ambient temperature for this test. Samples will be analyzed by UGA in this manner on each Analysis Day outlined in Table 2. Analytical Data. The UGA measures the partial pressures in a single sample aliquot over a set mass range of 0-105 atomic mass units (AMU) [Figure 2]; this set range was selected to slightly exceed the mass of the highest-mass expected reaction product (H2SO4). The Baratron complements the UGA by measuring the total pressure in the headspace of a sample vial. Coupled together, the quantitative abundances of gases will be monitored throughout the test. UGA analyses of the triplicate samples for each storage temperature, day, and simulant composition will be averaged, and standard deviations for each will be calculated. The compositions of starting species (shown in Table 1) will be characterized as a function of time, and the presence of any new compounds (reaction products) will be monitored as well. Total pressures will be recorded for each sample analysis, and any samples that show signs of leakage (e.g., a significant reduction in pressure or simulant volatiles) will be discarded. Anticipated Results. Testing is planned to begin in January 2022. The resulting data will allow compositional and phase changes in the volatile component of the simulants to be determined. Both the reduction in initial compounds and the addition of reaction products are expected to be observed. In addition, the relative efficacy of the different temperatures at pre-serving the initial composition of the simulants will be quantified. Finally, the regolith component of each sample will be argon-purged and stored in a controlled environment for future laboratory analysis. Compositional and morphological changes in the regolith are expected for samples above 0°C. This test will be repeated three times over the course of 2022. Understanding the effect of temperature on both the volatile and regolith components of analog lunar materials will allow requirements for a cold stowage freezer to be developed. The implementation of cold stowage for lunar polar missions will maximize the preservation of returned samples, enabling ground-breaking lunar and Solar System volatiles science for decades to come.

J L Mitchell↗

DOE OSTI2023

Observation of Same-Sign W W Production from Double Parton Scattering in Proton-Proton Collisions at s = 13 TeV

The first observation of the production of W$^\pm$W$^\pm$ bosons from double parton scattering processes using same-sign electron-muon and dimuon events in proton-proton collisions is reported. The data sample corresponds to an integrated luminosity of 138 fb$^{-1}$ recorded at a center-of-mass energy of 13 TeV using the CMS detector at the CERN LHC. Multivariate discriminants are used to distinguish the signal process from the main backgrounds. A binned maximum likelihood fit is performed to extract the signal cross section. The measured cross section for production of same-sign W bosons decaying leptonically is 80.7 $\pm$ 11.2 (stat) $^{+9.5}_{-8.6}$ (syst) $\pm$ 12.1 (model) fb, whereas the measured fiducial cross section is 6.28 $\pm$ 0.81 (stat) $\pm$ 0.69 (syst) $\pm$ 0.37 (model) fb. The observed significance of the signal is 6.2 standard deviations above the background-only hypothesis.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗