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DOE OSTI2019

Computer–aided process intensification: Challenges, trends and opportunities

Chemicals based products and the processes that manufacture them play important roles in sustaining our society. Chemical, biochemical, petrochemical and related processes are characterized by either conversion of specific raw materials to desired chemicals or extraction of desired chemicals from specific raw materials. Well–known examples in the first category are the conversion of methanol and acetic acid to form methyl acetate and water, and, carbon dioxide hydrogenation to methanol via the reverse water gas shift reaction. In the second category, the use of de–methanizer, de–ethanizer, de–propanizer, and so on, separation steps in gas processing plants are well–known. In the conversion–based processes, as the conversions of raw materials are usually not 100% complete, energy intensive downstream separation techniques need to be employed to separate the desired products and recycle the unreacted raw materials. Note that the conversion process itself may also be energy intensive. In the extraction–based processes where product chemicals do not usually represent 100% of the raw material, energy intensive separation techniques are commonly employed to achieve the desired separations. This means that for both categories of processes, energy in different forms need to be supplied and the processes during operation have the potential to produce waste that may lead to negative environmental impacts and cause supply chain issues. Furthermore, planet earth is facing challenges with respect to energy, water, food, and environment, and significant improvements in process efficiencies of new and/or existing processes are needed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Catalytic Activation of Polyethylene Model Compounds Over Metal-Exchanged Beta Zeolites

Decomposition of polymers by heterogeneous catalysts presents a promising approach for reuse of waste plastics. Here, we demonstrated non-hydrogenative decomposition of model polyolefins over proton-form and metal (Cu, Ni) ion-exchanged beta zeolites at moderate temperatures (ca. 300 degrees C). Near complete polyolefin decomposition was observed in batch reactions monitored by thermogravimetric analysis, while decomposition at partial conversion was studied in flow reactions. Ni-exchanged zeolites produced H 2 at substantially higher rates (> 10x) than other catalysts while also uniquely resisting deactivation over time. Application of the delplot formalism offered insights into the reaction network for polyolefin decomposition over Ni/BEA, most notably that H 2 is solely a primary product. We deduce that H 2 production is catalyzed by activation of C-H bonds at ionic Ni sites, and H 2 prevents buildup of polyaromatic coke species in Ni-exchanged zeolites that deactivate Cu-exchanged and protonic zeolites.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2012

Release of aged contaminants from weathered sediments: Effects of sorbate speciation on scaling of reactive transport

Hanford sediments impacted by hyperalkaline high level radioactive waste have undergone incongruent silicate mineral weathering concurrent with contaminant uptake. In this project, we studied the impact of background pore water (BPW) on strontium, cesium and iodine desorption and transport in Hanford sediments that were experimentally weathered by contact with simulated hyperalkaline tank waste leachate (STWL) solutions. Using those lab-weathered Hanford sediments (HS) and model precipitates formed during nucleation from homogeneous STWL solutions (HN), we (i) provided thorough characterization of reaction products over a matrix of field-relevant gradients in contaminant concentration, partial pressure of carbon dioxide, and reaction time; (ii) improved molecular-scale understanding of how sorbate speciation controls contaminant desorption from weathered sediments upon removal of caustic sources; and (iii) developed a mechanistic, predictive model of meso- to field-scale contaminant reactive transport under these conditions. In this final report, we provide detailed descriptions of our results from this three-year study, completed in 2012 following a one-year no cost extension.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2016

CRADA/NFE-15-05761 Report: Additive Manufacturing of Isotropic NdFeB Bonded Permanent Magnets

The technical objective of this technical collaboration phase I proposal is to fabricate net shape isotropic NdFeB bonded magnets utilizing additive manufacturing technologies at the ORNL MDF. The goal is to form complex shapes of thermoplastic and/or thermoset bonded magnets without expensive tooling and with minimal wasted material. Two additive manufacturing methods; the binder jet process; and big area additive manufacturing (BAAM) were used. Binder jetting produced magnets with the measured density of the magnet of 3.47 g/cm 3 , close to 46% relative to the NdFeB single crystal density of 7.6 g/cm 3 were demonstrated. Magnetic measurements indicate that there is no degradation in the magnetic properties. In addition, BAAM was used to fabricate isotropic near-net-shape NdFeB bonded magnets with magnetic and mechanical properties comparable or better than those of traditional injection molded magnets. The starting polymer magnet composite pellets consist of 65 vol% isotropic NdFeB powder and 35 vol% polyamide (Nylon-12). The density of the final BAAM magnet product reached 4.8 g/cm 3 , and the room temperature magnetic properties are: Intrinsic coercivity Hci = 8.65 kOe, Remanence Br = 5.07 kG, and energy product (BH) max = 5.47 MGOe (43.50 kJ/m 3 ). This study provides a new pathway for preparing near-net shape bonded magnets for various magnetic applications.

36 MATERIALS SCIENCE↗

NASA NTRS1974

Powder pressing in a macrosonic field

An investigation was conducted to extend the technology of powder product manufacturing to new forms and sizes, to improve their quality as well as pressing efficiency and to reduce waste. In the course of metal and nonmetal powder briquette pressing, macrosounds were associated with the external static pressing force, which led to an increase in the relative height, density and physicomechanical characteristics of the briquettes. This method permits the extension of the range of products that can be manufactured from powders and the improvement of their quality.

Protipopescu, A.↗

NASA NTRS1973

Investigation of water quality parameters at selected points on the Tennessee River

Physical, chemical, and biological water quality parameters have been investigated at the Widow's Creek steam plant. The water quality parameters and field site locations have been selected so as to be compatible with the interests and needs of the Environmental Application Office at Marshall Space Flight Center. All sampling and testing was conducted as directed in the 13th Edition of Standard Methods of Analysis for Water and Waste Water or as suggested by NASA'S Technical Officer. Data is presented in a form compatible with that presently being collected by other agencies.

Manger, M. C.↗

NASA NTRS1983

The Antaeus Project - An orbital quarantine facility for analysis of planetary return samples

A design is presented for an earth-orbiting facility for the analysis of planetary return samples under conditions of maximum protection against contamination but minimal damage to the sample. The design is keyed to a Mars sample return mission profile, returning 1 kg of documented subsamples, to be analyzed in low earth orbit by a small crew aided by automated procedures, tissue culture and microassay. The facility itself would consist of Spacelab shells, formed into five modules of different sizes with purposes of power supply, habitation, supplies and waste storage, the linking of the facility, and both quarantine and investigation of the samples. Three barriers are envisioned to protect the biosphere from any putative extraterrestrial organisms: sealed biological containment cabinets within the Laboratory Module, the Laboratory Module itself, and the conditions of space surrounding the facility.

Sweet, H. C.↗

NASA NTRS2005

Control of Effluent Gases from Solid Waste Processing Using Carbon Nanotubes

One of the major problems associated with solid waste processing technologies is the release of effluent gases and contaminants that are in gaseous formed from the processes. A number of other gases, in particular NO(x), SO2, NH3, Hydrocarbons (e.g. CH4) do present hazards to the crew in space habitats. Reduction of mass, power, volume and resupply can be achieved by using catalyst impregnated carbon nanotubes as compared to other catalytic systems. The development and characterization of an innovative approach for the control and elimination of gaseous toxins using single walled carbon nanotubes (SWNTs) promise superior performance over conventional approaches. This is due to the ability to direct the selective uptake of gaseous species based on their controllable pore size, high adsorptive capacity and the effectiveness of carbon nanotubes as catalyst supports for gaseous conversion. For example, SWNTs have high adsorptive capacity for NO and the adsorbed NO can be decomposed to N2 and O2 . Experimental results showing the decomposition of NO on metal impregnated carbon nanotubes is presented. Equivalent System Mass (ESM) comparisons are made of the existing TCCS systems with the carbon nanotube technology for removing NO(x). The potential for methane decomposition using carbon nanotubes catalysts is also discussed.

Fisher, John↗

NASA NTRS1999

Electrochemical production of ozone and hydrogen peroxide

Methods of using ozone have been developed which sterilize instruments and medical wastes, oxidize organics found in wastewater, clean laundry, break down contaminants in soil into a form more readily digested by microbes, kill microorganisms present in food products, and destroy toxins present in food products. The preferred methods for killing microorganisms and destroying toxins use pressurized, humidified, and concentrated ozone produced by an electrochemical cell.

Murphy, Oliver J.↗

NASA NTRS2002

Method of sterilization using ozone

Methods of using ozone have been developed which sterilize instruments and medical wastes, oxidize, organics found in wastewater, clean laundry, break down contaminants in soil into a form more readily digested by microbes, kill microorganisms present in food products, and destroy toxins present in food products. The preferred methods for killing microorganism and destroying toxins use pressurized, humidified, and concentrated ozone produced by an electrochemical cell.

Murphy, Oliver J.↗

NASA NTRS2014

Geologic Mapping of Vesta

We report on a preliminary global geologic map of Vesta, based on data from the Dawn spacecraft's High- Altitude Mapping Orbit (HAMO) and informed by Low-Altitude Mapping Orbit (LAMO) data. This map is part of an iterative mapping effort; the geologic map has been refined with each improvement in resolution. Vesta has a heavily-cratered surface, with large craters evident in numerous locations. The south pole is dominated by an impact structure identified before Dawn's arrival. Two large impact structures have been resolved: the younger, larger Rheasilvia structure, and the older, more degraded Veneneia structure. The surface is also characterized by a system of deep, globe-girdling equatorial troughs and ridges, as well as an older system of troughs and ridges to the north. Troughs and ridges are also evident cutting across, and spiraling arcuately from, the Rheasilvia central mound. However, no volcanic features have been unequivocally identified. Vesta can be divided very broadly into three terrains: heavily-cratered terrain; ridge-and-trough terrain (equatorial and northern); and terrain associated with the Rheasilvia crater. Localized features include bright and dark material and ejecta (some defined specifically by color); lobate deposits; and mass-wasting materials. No obvious volcanic features are evident. Stratigraphy of Vesta's geologic units suggests a history in which formation of a primary crust was followed by the formation of impact craters, including Veneneia and the associated Saturnalia Fossae unit. Formation of Rheasilvia followed, along with associated structural deformation that shaped the Divalia Fossae ridge-and-trough unit at the equator. Subsequent impacts and mass wasting events subdued impact craters, rims and portions of ridge-and-trough sets, and formed slumps and landslides, especially within crater floors and along crater rims and scarps. Subsequent to the formation of Rheasilvia, discontinuous low-albedo deposits formed or were emplaced; these lie stratigraphically above the equatorial ridges that likely were formed by Rheasilvia. The last features to be formed were craters with bright rays and other surface mantling deposits. Executed progressively throughout data acquisition, the iterative mapping process provided the team with geologic proto-units in a timely manner. However, interpretation of the resulting map was hampered by the necessity to provide the team with a standard nomenclature and symbology early in the process. With regard to mapping and interpreting units, the mapping process was hindered by the lack of calibrated mineralogic information. Topography and shadow played an important role in discriminating features and terrains, especially in the early stages of data acquisition.

Vesta↗

DOE OSTI2012

Release of Aged Contaminants from weathered sediments: Effects of sorbate speciation on scaling of reactive transport

Hanford sediments impacted by hyperalkaline high level radioactive waste have undergone incongruent silicate mineral weathering concurrent with contaminant uptake (Chorover et al., 2008). In this project, we studied the impact of background pore water (BPW) on strontium, cesium and iodine desorption and transport in Hanford sediments that were experimentally weathered by contact with simulated hyperalkaline tank waste leachate (STWL) solutions. Using those lab-weathered Hanford sediments (HS) and model precipitates formed during nucleation from homogeneous STWL solutions (HN), we (i) provided thorough characterization of reaction products over a matrix of field-relevant gradients in contaminant concentration, P CO2 , and reaction time; (ii) improved molecular-scale understanding of how sorbate speciation controls contaminant desorption from weathered sediments upon removal of caustic sources; and (iii) developed a mechanistic, predictive model of meso- to field-scale contaminant reactive transport under these conditions. Below, we provide some detailed descriptions of our results from this three year study, recently completed following a one-year no cost extension.

Chorover, Jon↗

DOE OSTI2020

Carbon electrodes based capacitive deionization for the desalination of water

A capacitive deionization system includes first and second electrodes comprising tire derived carbon particles obtained from a carbonaceous waste-tire source material containing carbon black. A conductive polymer coating on the carbon particles forms coated carbon particles. The first electrode and the second electrode define a flow channel there between, having a first opening for conducting saline solution into the flow channel and a second opening for conducting treated saline solution from the flow channel. A first current collector is provided for the first electrode and a second current collector is provided for the second electrode. An electrical connection between the first and second electrodes. A method of making a system for the capacitive deionization of a salt from a liquid, and a method for the capacitive desalination of a saline solution are also disclosed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2015

Success in commissioning a key U.S. radioactive waste burial site through the technical support of Dufrane Nuclear Shielding Incorporated (DNSI) - 15476

With the -phase out- of the South Carolina based Barnwell Radioactive Waste Burial Site, and the stockpile and storage of radioactive waste and irradiated components throughout the U.S. Nuclear Industry for decades, the opening of the Texas Low-Level Radioactive Waste Disposal Compact Facility by Waste Control Specialists (WCS), is a game changer in solving this industry-wide issue. For the first time in decades, generators now have the opportunity to send their waste to a site specifically designed to permanently sequester the waste in a licensed facility that will protect public health and the environment, better than any built to date. As history has shown through the many decades of the U.S. Commercial and Federal Nuclear Industry, site operators and management have relied heavily on contractors and vendors with exceptional expertise and decades of experience to achieve success and meet their goals. The commissioning of WCS was no exception as DNSI was contracted to design, develop, build and deploy a major component required for the opening and successful operation of the WCS site. This component, being the Modular Concrete Canister (MCC), is the -work horse- of the site. With its enormous size, weight and strength, it provides many functions that meet and comply with the site performance assessment (PA) under 10 CFR Part 61, the site WAC, and Texas Low-Level Radioactive Waste Disposal Authority. Offsite contracting the production and delivery of this critical component was a major step toward success in meeting schedule and cost for the much needed opening of the Texas Compact and Federal site. In selecting a shielding vendor, WCS partnered with a U.S. Nuclear Service company with over 30 years of experience which spans the entire U.S. Commercial, Federal, and Nuclear Industry. The task given DNSI was not a simple one, it involved every aspect from start to finish of the design, production and delivery of rectangular, cylindrical and -irradiated hardware- (IH) MCCs, that could accept waste up to 100 Sv /Hr contact dose rates. The enormity of this project was quite clear and required extensive quality control, construction of batch plants, purchase of huge quantities of raw materials, setting up a production site in a neighboring city, relocation of personnel from company headquarters, and safely transporting 8,000 Tons of MCC components 75 miles one-way on West Texas highways daily. Most important of all, this was accomplished safely with no incidents, no component failures or rejects, and on schedule. The start of receipt, of -in-compact waste- and -out-of-compact waste- was conducted virtually in a 3 month period time span. To help guarantee success and quality of product, all forms had surfaces machined, heavy duty elastomer coatings were applied to concrete surfaces, only galvanized anchors were used, and the batch plant was run to strict ASME standards thus testing every 50 cubic yards of concrete poured. With significant teamwork and success from Vendors such as DNSI, WCS and the Texas Compact has evolved as one of the leading radioactive waste sites in the U.S. and the world, providing safe, secure and compliant permanent waste disposal services by using technical expertise and innovation of the highest standards. (authors)

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DOE OSTI2018

Test Bed: Treatability of Hanford Tank Waste - 18501

In an effort to advance the Low Activity Waste Pretreatment System technology readiness level at the Hanford Site, the effectiveness of a critical technology element, sRF ion-exchange resin, was demonstrated in the selective removal of Cs-137 from 11.5 L of composited Hanford supernate tank waste. Prior to ion-exchange, solids filtration was performed on the tank waste composite. Between the time of filtrate collection and filtrate processing on the ion-exchange columns, additional solids had formed. These secondary solids resulted from the combination of supernates high in fluoride content with supernates high in phosphate content and the relatively short blend time. Samples were collected before, during and after the ion-exchange process for characterization of a full suite of constituents (inorganic, organic, and radionuclides) to aid in the classification of the cesium-removed waste for shipping, receiving, treatment, and disposal determinations. Following chemical analysis, the remaining 10.8 L (2.9 gal) of cesium-depleted waste was shipped to an off-site vendor for grout-encapsulation and eventual disposal at the Waste Control Specialists Federal Waste Disposal Facility in Andrews, Texas as low-level waste. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2015

Limitation of tritium outgassing from tritiated solid waste drums

In the framework of the development of fusion thermonuclear reactors, tritiated solid waste is foreseen and will have to be managed. The management of tritiated waste implies limitations in terms of activity and tritium degassing. The degassing tritium can be under the form of tritiated hydrogen, tritiated water and, in some specific cases, negligible amount of tritiated volatile organic compound. Hence, considering the major forms of degassing tritium, CEA has developed a mixed-compound dedicated to tritium trapping in drums. Based on several experiments, the foreseen mixed compound is composed of MnO{sub 2}, Ag{sub 2}O, Pt and molecular sieve, the three first species having the ability to convert tritiated hydrogen into tritiated water and the last one acting as a trap for tritiated water. To assess the performance of the trapping mixture, experimental tests were performed at room temperature on tritiated dust composed of beryllium and carbon. It was shown that the metallic oxides mixture used for tritiated hydrogen conversion is efficient and that tritiated water adsorption was limited due to an inefficient regeneration of the molecular sieve prior to its use. Apart from this point, the tritium release from waste was reduced by a factor of 5.5, which can be improved up to 87 if the adsorption step is efficient.

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DOE OSTI2017

Comparison of Exhibited Wear in Tefzel?, Kynar?, and UHMWPE Valve Seats Exposed to Cyclic Operations with Abrasive Slurry - 17519

Pacific Northwest National Laboratory (PNNL) conducted abrasive-wear testing of ball valves used for double valve isolation in nuclear waste process lines. The valve seat materials consisted of Kynar{sup R}, Tefzel{sup R}, and ultra-high-molecular-weight polyethylene (UHMWPE). Cycle testing was conducted for 1500 operating cycles for the Kynar{sup R} and Tefzel{sup R} valve seats and 5500 cycles for the UHMWPE valve seats. A valve operational cycle consisted of slurry flow, slurry gravity drain, flush water flow, and flush water gravity drain. Both two-way and three-way valves were evaluated, and valves were configured in simulated manifolds so the impact of serving various operational functions (e.g., slurry, flush, or drain control) could be evaluated as some valves are flushed prior to being cycled and others are not. Testing was conducted in PNNL's Multi-Phase Transport Evaluation Loop Facility using a performance-based simulant developed by PNNL specifically for this test program to emulate abrasive slurries for Hanford Tank Farms Waste Transfer System during single-shell tank retrieval and waste feed delivery to the Hanford Tank Waste Treatment and Immobilization Plant. Pre- and post-test valve tear-down evaluations were conducted to observe changes in the condition of internal components for the various seat materials. The various forms of physical wear observed for the different seat materials are presented. The wear results can be used to assess seat materials and valve configurations for application to waste transfer operations, and the observed wear mechanisms can provide insight into assessing valve service life. This information will be used to identify and select additional valve designs that should be evaluated for certification for future use. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2019

Analysis of the Impact of Radiation on Cameras and Robotic Perception - 19242

Robotic systems are increasingly used for inspection, maintenance, and disaster assistance for nuclear power plants. These robots utilize increasingly high levels of autonomy to operate in environments that are unsafe for humans to operate the robot in or require more precise control over the robot than a human can offer. In these cases, the robot must include perception and computation components to autonomously sense and navigate through the environment to fulfill its mission. This difficult task is complicated by radiation interfering with sensors' operation. The impact of this interference is largely unexplored, as existing works on radiation interference on sensors focus on estimating the incident radiation, rather than how it impacts a robotic system using the sensor. In this work, we seek to quantify and describe the impact of radiation on cameras, and how the radiation affects robotic performance. In this paper we study cameras that are suitable for small, lightweight unmanned aerial vehicles (UAVs) that are increasingly deployed to fly in confined areas in emergencies, where the surrounding environment is unsafe for workers to operate. These small UAVs lack the payload capacity to carry significant radiation shielding, so any onboard sensors will be affected by radiation. In the case of cameras, this radiation appears as noise in the camera imagery. This noise will interfere with the UAV's operation, by obscuring obstacles and interfering with localization and optical flow algorithms that detect detailed features in the environment. To date, there is a lack of information on how the radiation noise in the camera image impacts the overall robot system performance Existing work focuses on estimating the amount of incident radiation by measuring the corruption in the images. However, these works suffer several shortcomings for robotic systems. First, a robot must be able to successfully navigate its environment during a successful mission, and merely quantifying the amount of radiation noise in an image does not adequately explain how it may interfere with higher level navigation and perception tasks. Second, radiation estimation procedures rely on focusing the camera on a known and static background. This is unsuitable for robotic exploration tasks, where the robot frequently moves around an unknown environment that may be dynamically changing. Our work contains two contributions that address these shortcomings. First, we conduct a detailed analysis of the noise radiation causes in cameras by exposing cameras that are commonly used on UAVs [e.g., small form factor complementary metal-oxide-semiconductor (CMOS) cameras] to varying levels of radiation that may be present in emergency scenarios. From this exposure, we quantify not only how much noise is present, but quantify its appearance. By quantifying the appearance and amount of noise in a camera image, researchers can design mitigation strategies for the corruption, so that their robotic systems can operate in these challenging environments. Second, we demonstrate how to leverage this experimental data in robotic simulations. Using data from the first set of experiments allows us to test and verify the robots in simulation. Using simulators allows us to verify the robots will perform as expected during critical times without needing expensive test equipment or damaging valuable robot prototypes. Other researchers using robots for exploration of irradiated environments will benefit from our research by incorporating similar noise models in their research. 1 Southwest Research Institute{sup R} is a registered trademark of Southwest Research Institute in the United States and/or other countries. This will increase the reliability of robotic systems prior to deployment in emergency situations, which will in turn increase their effectiveness and speed the development of robots that would otherwise need expensive and time-consuming test procedures to validate. (authors)

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