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DOE OSTI2018

Safety Evaluation of Nitric Acid Reactions with Polysaccharides

The hazards of polysaccharides in a transuranic (TRU) waste drum exposed to nitric acid (HNO3) and metal nitrate salts have been evaluated, based on considerations of how complex nitrogen redox cycles carry out the aqueous phase oxidation of alcohols and related organic functional groups. Of particular emphasis is how these exothermic reactions, coupled with a positive feedback loop inherent to nitrogen redox chemistry, can initiate an autocatalytic thermal runaway and explosive gas generation. This poses the most significant hazard for a TRU waste drum under ambient conditions where acidic solution may be present, either in small quantities as free liquid or sorbed within a solid matrix. Regarding specific mechanistic details, nitric acid is an extremely potent oxidant but is remarkably inert, rarely interacting directly with oxidizable substrates, instead exerting its vast potential energy through lower oxidation state reactants such as nitrogen dioxide (NO 2 ) and nitrous acid (HNO 2 ). These lower oxidation states of nitrogen are generated from the slow self-decomposition of nitric acid, as a result of which oxidation reactions involving nitric acid that have not been preloaded with these reactants commonly experience a quiescent induction period. It is the end of this induction period when exothermic reactivity increases rapidly that the system is most vulnerable to autocatalytic thermal runaway. Metal nitrate salts promote this ambient temperature solution chemistry (cf. traditional oxidizer properties of metal nitrate salts, which operate in the solid state at elevated temperatures) by releasing nitric acid into the system. Although less reactive than alcohols by virtue of extensive hydrogen bonding, carbohydrates are oxidized by nitric acid through the same fundamental mechanisms, potentially proceeding through a series of oxidation steps. For polymeric carbohydrates (polysaccharides) the chemistry is complicated by a variety of competing side reactions, including acid-catalyzed hydrolytic depolymerization to more reactive (ultimately monomeric) units, as well as other degradation reactions promoted by radical mechanisms. For this reason, polysaccharides that are more susceptible to hydrolysis such as starches are more reactive than cellulose, with the attendant microbial population in starch based kitty litter adding a special aspect of reactivity. A spectrum of nitrogen containing gas products is generated from polysaccharide oxidation by nitric acid depending on the reaction conditions - for example, fuel lean mixtures tend towards producing more oxidized gases such as NO 2 , and thus favor an autocatalytic cycle, relative to fuel rich conditions that produce lower oxidation state gases such as nitrous oxide (N 2 O). These nitrogen based gases may be accompanied by variable quantities of carbon dioxide (CO 2 ), which may be generated from small molecule (e.g., oxalic acid) oxidation or from decarboxylation of previously oxidized functional groups.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2019

Safety Evaluation of Nitric Acid Reactions with Polysaccharides

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2023

Carbon Fiber and Polymer Composites

Tooling is an integral part of composites manufacturing. Composite tools, also called ‘soft’ tools, are more easily constructed than ‘hard’ metal tools and, because they are made from materials similar to the manufactured composite part, they can be made in-house and have a good co-efficient of thermal expansion match. However, as the ‘soft’ designation suggests, they are more vulnerable to wear and typically find application in relatively low-volume production. Additive manufacturing of thermoplastics has proven to be a lucrative option that can help improve the tooling functionalities, as it offers more design flexibility. Owing to the inherent nature of additive manufacturing, the possibility of printing sensors within the tool material and at proximity to otherwise inaccessible areas of the tool become a reality. Continuous carbon fiber (CCF)-reinforced three-dimensional (3D) printing of engineering thermoplastics has proven to be a viable option to strengthen a part well beyond the ideal moduli of unmodified thermoplastic. Furthermore, adding nanotubes or graphene to the thermoplastic matrix will also improve both the thermal conductivity and interlaminar shear strength within the tool. Carbon nanotubes (CNTs) and carbon fibers (CFs) are microwave susceptors; exploiting the physics of Joule heating to increase the energy efficiency of tool hardening and cure rates is a core goal of this project. Because of the rapid volumetric heating enabled by the absorption of microwave or radio frequency energy and electromagnetic (EM) annealing presents an attractive opportunity to significantly reduce manufacturing cycle times while improving part performance.

Craps, Matthew G.↗

DOE OSTI2019

Understanding Nitrate Chemistry - The Key to Safer and More Efficient TRU Waste Acceptance - 19618

Investigations into the Waste Isolation Pilot Plant (WIPP) radiological release from a transuranic (TRU) waste drum concluded that the event was initiated by a thermal runaway, principally involving interactions between the polysaccharide-based kitty litter and nitric acid, which released radiological material along with hot gases and combustible materials from the drum. In this paper, the hazards of polysaccharides present as either starch based kitty litter or cellulose rags in a TRU waste drum exposed to nitric acid (and by extension metal nitrate salts) have been evaluated, based on considerations of how complex nitrogen redox cycles carry out the aqueous phase oxidation of alcohols and related organic functional groups. These exothermic reactions, coupled with a positive feedback loop inherent to nitrogen redox chemistry, can initiate an autocatalytic thermal runaway and explosive gas generation, which poses the most significant risk under ambient conditions where acidic solution may be present (in small quantities as free liquid or sorbed within a solid matrix). Nitric acid is an extremely potent oxidant but is itself remarkably inert, rarely interacting directly with oxidizable substrates and instead exerting its vast potential energy through lower oxidation state reactants such as nitrogen dioxide and nitrous acid that are generated from its slow self-decomposition. Nitrous acid is the reactant that carries out substrate oxidation, and systems that are not pre-loaded with nitrous acid will experience an induction period before significant reactivity commences. Under oxidizing fuel-lean conditions, nitrogen dioxide may induce autocatalytic nitrous acid formation, which may supplement additional side-reactions, potentially leading to thermal runaway. Therefore, the system is most vulnerable at the end of an induction period. Metal nitrate salts promote this ambient temperature solution chemistry (cf. traditional oxidizer properties of metal nitrate salts, which operate in the solid state at elevated temperatures) by releasing nitric acid into the system via hydrolysis. Unlike simple alcohols with a single hydroxyl functional group, the chemistry of polymeric carbohydrates (polysaccharides) such as starches and cellulose is more diverse. Therefore, the oxidation of the simple monomeric carbohydrate glucose is first examined to provide insight into the analogous reactivity with polysaccharides. Although less reactive than alcohols by virtue of extensive hydrogen bonding, carbohydrates are oxidized by nitric acid through the same fundamental mechanisms, complicated by a variety of competing side reactions including acid-catalyzed hydrolytic depolymerization to more reactive (ultimately monomeric) units, as well as other degradation reactions promoted by radical mechanisms. For this reason, polysaccharides such as starches that are more susceptible to hydrolysis are more reactive than cellulose, with the attendant microbial population in starch based kitty litter adding a special aspect of reactivity. From this safety evaluation, a bounding latency period has been developed beyond which a stored TRU waste drum that contains polysaccharides (starch based kitty litter excluded) commingled with nitric acid and/or metal nitrate salts may no longer present a hazard under ambient conditions, based on a compilation of induction periods and reaction times involving nitric acid with various oxidizable substrates under a variety of conditions from synthetic procedures, tests, and adverse incident scenarios. By obviating the need for costly treatment options or characterization, a better understanding of nitrate redox chemistry and the hazards it presents with polysaccharide oxidation thus provides a more efficient means to safely dispose of TRU waste generated within the Department of Energy (DOE) complex. (author)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2017

Oxidation Behavior of Matrix Graphite and Its Effect on Compressive Strength

Matrix graphite (MG) with incompletely graphitized binder used in high-temperature gas-cooled reactors (HTGRs) is commonly suspected to exhibit lower oxidation resistance in air. In order to reveal the oxidation performance, the oxidation behavior of newly developed A3-3 MG at the temperature range from 500 to 950°C in air was studied and the effect of oxidation on the compressive strength of oxidized MG specimens was characterized. Results show that temperature has a significant influence on the oxidation behavior of MG. The transition temperature between Regimes I and II is ~700°C and the activation energy ( E a ) in Regime I is around 185 kJ/mol, a little lower than that of nuclear graphite, which indicates MG is more vulnerable to oxidation. Oxidation at 550°C causes more damage to compressive strength of MG than oxidation at 900°C. Comparing with the strength of pristine MG specimens, the rate of compressive strength loss is 77.3% after oxidation at 550°C and only 12.5% for oxidation at 900°C. Microstructure images of SEM and porosity measurement by Mercury Porosimetry indicate that the significant compressive strength loss of MG oxidized at 550°C may be attributed to both the uniform pore formation throughout the bulk and the preferential oxidation of the binder.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2022

Resilient Operating Constraints for Power Distribution Systems under Setpoint Attacks

Integration and operation of distributed generation (DG) and energy storage (ES) in power distribution systems are enabled by communication networks and embedded sensor and control devices that increase the vulnerability of the systems to cyber-threats, broadening the attack surface and making adversary actions more unpredictable. This paper proposes a methodology that uses ellipsoidal approximations to quantify the potential damage caused by successful attacks that affect, directly or indirectly, the desired operation setpoints and may drive the power distribution operation to unsafe states by violating the limits of voltage or line flows. More specifically, a new methodology is introduced to find the optimal non-symmetric operating constraints that can be imposed to each DG and ES in order to guarantee that the power distribution system is resilient to any malicious setpoints. The proposed method takes as inputs the system topology, DG and ES capabilities, and load limits to solve a convex optimization problem formulated using linear matrix inequalities (LMIs) and the power flow equations. The proposed solution is agnostic to the attacker's action or load profile and it does not require any assumption about the location or means of the attack. The numerical results on a test distribution feeder with several DG and ES illustrate how the proposed resilient operating constraints guarantee the security of the power distribution system under setpoint attacks.

Giraldo, Jairo↗

DOE OSTI2021

User Role Identification in Software Vulnerability Discussions over Social Networks

Understanding and early awareness of software vulnerabilities is vital for preventing and mitigating potential impacts from cybersecurity events. One step toward early characterization of software vulnerabilities may involve analyzing discussion and spread of information in online social networks. Prior work has used information from such discussions over multiple online forums to develop dynamic networks among users followed by analysis of structure, spread, and information evolution. In this work, we advance the state-of-the-art by focusing on data-driven learning of types, roles, and transition of roles exhibited by users over time. In social networks, users take on particular roles based on their actions and structure of the network. Identifying “meaningful” roles can help separate potential users of interest from the larger community, and identify patterns in a network. We will identify and compare roles found in online forums (e.g., Twitter) using techniques such as feature-based Non-negative Matrix Factorization coupled with topological and influence-based measures of centrality. Since users’ activities change over time, we also analyze role evolution in dynamic networks.

Jones, Rebecca D.↗

DOE OSTI2015

Interdisciplinary research in climate and energy sciences

Due to the complex nature of climate change, interdisciplinary research approaches involving knowledge and skills from a broad range of disciplines have been adopted for studying changes in the climate system as well as strategies for mitigating climate change (i.e., greenhouse gas emissions reductions) and adapting to its impacts on society and natural systems. Harnessing of renewable energy sources to replace fossil fuels is widely regarded as a long-term mitigation strategy that requires the synthesis of knowledge from engineering, technology, and natural and social sciences. In this study, we examine how the adoption of interdisciplinary approaches has evolved over time and in different geographic regions. We conducted a comprehensive literature survey using an evaluation matrix of keywords, in combination with a word cloud analysis, to evaluate the spatiotemporal dynamics of scholarly discourse about interdisciplinary approaches to climate change and renewable energy research and development (R&D). Publications that discuss interdisciplinary approaches to climate change and renewable energy have substantially increased over the last 60 years; it appears, however, that the nature, timing, and focus of these publications vary across countries and through time. Over the most recent three decades, the country-level contribution to interdisciplinary research for climate change has become more evenly distributed, but this was not true for renewable energy research, which remained dominated by the United Sates and a few other major economies. The research topics have also evolved: Water resource management was emphasized from 1990s to 2000s, policy and adaptation were emphasized from the 2000s to 2010 – 2013, while vulnerability became prominent during the most recent years (2010 – 2013). Lastly, our analysis indicates that the rate of growth of interdisciplinary research for renewable energy lags behind that for climate change, possibly because knowledge emanating from climate change science has motivated the subsequent upswing in renewable energy R&D.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS2011

A Method of Strengthening Composite/Metal Joints

The term tape setback method denotes a method of designing and fabricating bonded joints between (1) box beams or other structural members made of laminated composite (matrix/ fiber) materials and (2) metal end fittings used to fasten these structural members to other structural members. The basic idea of the tape setback method is to mask the bonded interface between the metallic end fitting and composite member such that the bond does not extend out to the free edges of the composite member. The purpose served by the tape setback method is to strengthen the joints by decoupling stress concentrations from edge defects, which can cause premature failures. A related prior method that serves a similar purpose, involving the use of tapered adherends at the joints, can be too difficult and costly to be acceptable in some applications. The tape setback method offers an easier, less costly alternative. The structural members to which the method was originally applied were box beams in the form of composite tubes having flat faces with rounded corners. The end fittings were plugs made of a low-thermal- expansion nickel/iron alloy (see figure). In computational-simulation studies of tensile and compressive loading of members without tape setback, stresses were found to be concentrated at the free end edges of the composite tubes, and inspection of members that had been subjected to real tension and compression tests showed that cracks started at the free end edges. As applied to these members, the tape setback method makes them less vulnerable to initiation of failure at edge defects produced during fabrication. In real tension tests of comparable members without and with tape setback, the average mean tensile strength of the members with tape setback was found to be 1.9 times that of the members without tape setback.

Polis, Daniel L.↗

NASA NTRS2007

Investigation of MMOD Impact on STS-115 Shuttle Payload Bay Door Radiator

The Orbiter radiator system consists of eight individual 4.6 m x 3.2 m panels located with four on each payload bay door. Forward panels #1 and #2 are 2.3 cm thick while the aft panels #3 and #4 have a smaller overall thickness of 1.3 cm. The honeycomb radiator panels consist of 0.028 cm thick Aluminum 2024-T81 facesheets and Al5056-H39 cores. The face-sheets are topped with 0.005 in. (0.127 mm) silver-Teflon tape. The radiators are located on the inside of the shuttle payload bay doors, which are closed during ascent and reentry, limiting damage to the on-orbit portion of the mission. Post-flight inspections at the Kennedy Space Center (KSC) following the STS-115 mission revealed a large micrometeoroid/orbital debris (MMOD) impact near the hinge line on the #4 starboard payload bay door radiator panel. The features of this impact make it the largest ever recorded on an orbiter payload bay door radiator. The general location of the damage site and the adjacent radiator panels can be seen in Figure 2. Initial measurements of the defect indicated that the hole in the facesheet was 0.108 in. (2.74 mm) in diameter. Figure 3 shows an image of the front side damage. Subsequent observations revealed exit damage on the rear facesheet. Impact damage features on the rear facesheet included a 0.03 in. diameter hole (0.76 mm), a approx.0.05 in. tall bulge (approx.1.3 mm), and a larger approx.0.2 in. tall bulge (approx.5.1 mm) that exhibited a crack over 0.27 in. (6.8 mm) long. A large approx.1 in. (25 mm) diameter region of the honeycomb core was also damaged. Refer to Figure 4 for an image of the backside damage to the panel. No damage was found on thermal blankets or payload bay door structure under the radiator panel. Figure 5 shows the front facesheet with the thermal tape removed. Ultrasound examination indicated a maximum facesheet debond extent of approximately 1 in. (25 mm) from the entry hole. X-ray examinations revealed damage to an estimated 31 honeycomb cells with an extent of 0.85 in. x 1.1 in. (21.6 x 27.9 mm). Pieces of the radiator at and surrounding the impact site were recovered during the repair procedures at KSC. They included the thermal tape, front facesheet, honeycomb core, and rear facesheet. These articles were examined at JSC using a scanning electron microscope (SEM) with an energy dispersive x-ray spectrometer (EDS). Figure 6 shows SEM images of the entry hole in the facesheet. The asymmetric height of the lip may be attributed to projectile shape and impact angle. Numerous instances of a glass-fiber organic matrix composite were observed in the facesheet tape sample. The fibers were approximately 10 micrometers in diameter and variable lengths. EDS analysis indicated a composition of Mg, Ca, Al, Si, and O. Figures 7 and 8 present images of the fiber bundles, which were believed to be circuit board material based on similarity in fiber diameter, orientation, consistency, and composition. A test program was initiated in an attempt to simulate the observed damage to the radiator facesheet and honeycomb. Twelve test shots were performed using projectiles cut from a 1.6 mm thick fiberglass circuit board substrate panel. Results from test HITF07017, shown in figures 9 and 10, correlates with the observed impact features reasonably well. The test was performed at 4.14 km/sec with an impact angle of 45 degrees using a cylindrical projectile with a diameter and length of 1.25 mm. The fiberglass circuit board material had a density of 1.65 g/cu cm, giving a projectile mass of 2.53 mg. An analysis was performed using the Bumper code to estimate the probability of impact to the shuttle from a 1.25 mm diameter particle. Table 1 shows a 1.6% chance (impact odds = 1 in 62) of a 1.25 mm or larger MMOD impact on the radiators of the vehicle during a typical ISS mission. There is a 0.4% chance (impact odds = 1 in 260) that a 1.25 mm or larger MMOD particle would impact the RCC wing leading edge and nose cap during a typical miion. Figure 11 illustrates the vulnerable areas of the wing leading edge reinforced carbon-carbon (RCC), an area of the vehicle that is very sensitive to impact damage. The highlighted red, orange, yellow, and light green areas would be expected to experience critical damage if impacted by an OD particle such as the one that hit the RH4 radiator panel on STS-115.

Hyde, J.↗

NASA NTRS2004

Response Of Mineralizing And Non-Mineralizing Bone Cells To Fluid Flow: An In Vitro Model For Mechanotransruction

Humans reach peak bone mass at age 30. After this point, we lose 1 to 2 percent of bone mass each decade. In the microgravity environment of space, astronauts lose bone mass at an accelerated rate of 1 to 2 percent each month. When astronauts travel to Mars, they may be in space for as long as 3 years. During this time, they may lose about half of their bone mass from weight-bearing bones. This loss may be irreversible. The drastic loss in bone that astronauts experience in space makes them much more vulnerable to fractures. In addition, the corresponding removal of calcium from bone results in higher levels of calcium in the blood, which increases the risk of developing kidney stones. Currently, studies are being conducted which investigate factors governing bone adaptation and mechanotransduction. Bone is constantly adapting in response to mechanical stimuli. Increased mechanical loading stimulates bone formation and suppresses bone resorption. Reduction in mechanical loading caused by bedrest, disuse, or microgravity results in decreased bone formation and possibly increased bone resorption. Osteoblasts and osteoclasts are the two main cell types that participate in bone remodeling. Osteoblasts are anabolic (bone-forming) cells and osteoclasts are catabolic (bone-resorbing) cells. In microgravity, the activity of osteoblasts slows down and the activity of osteoclasts may speed up, causing a loss of bone density. Mechanotransduction, the molecular mechanism by which mechanical stimuli are converted to biochemical signals, is not yet understood. Exposure of cells to fluid flow imposes a shear stress on the cells. Several studies have shown that the shear stress that results from fluid flow induces a cellular response similar to that induced by mechanical loading. Thus, fluid flow can be used as an in vitro model to simulate the mechanical stress that bone cells experience in vivo. Previous in vitro studies have shown that fluid flow induces several responses in osteoblasts, including increased proliferation, osteoblastic differentiation, alkaline phosphatase activity, and production of nitric oxide, prostaglandins, and osteopontin. Several proteins have been implicated in osteoblastic mechanotransduction including Bone Morphogenetic Protein-2 (BMP-2), parathyroid hormone, 1,25-dihydroxyvitamin D3 receptor, osteopontin (OPN), osteoprotegerin (OPG), and alkaline phosphatase (AP). We will characterize relative levels of each protein in mineralizing or non-mineralizing MC3T3 osteoblastic cells that have been exposed to fluid flow compared to non-fluid flow using immunofluorescent staining and two- photon laser microscopy as well as western blotting. Because calcium-mediated pathways are important in osteoblastic signaling, we will transfect MC3T3 cells with cameleon probes for Ca2+ containing YFP and CFP. Results will be analyzed using FRET/FLIM to study differential release of intracellular Ca(2+) in response to fluid flow and conditions inducing matrix mineralization. In addition, we plan to conduct several microarray experiments to determine differential gene expression in MC3T3 cells in response to fluid flow and conditions inducing mineralization.

Makuch, Lauren A.↗