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DOE OSTI2014

Determination of heat conductivity and thermal diffusivity of waste glass melter feed: Extension to high temperatures

The heat conductivity ({lambda}) and the thermal diffusivity (a) of reacting glass batch, or melter feed, control the heat flux into and within the cold cap, a layer of reacting material floating on the pool of molten glass in an all-electric continuous waste glass melter. After previously estimating {lambda} of melter feed at temperatures up to 680 deg C, we focus in this work on the {lambda}(T) function at T > 680 deg C, at which the feed material becomes foamy. We used a customized experimental setup consisting of a large cylindrical crucible with an assembly of thermocouples, which monitored the evolution of the temperature field while the crucible with feed was heated at a constant rate from room temperature up to 1100°C. Approximating measured temperature profiles by polynomial functions, we used the heat transfer equation to estimate the {lambda}(T) approximation function, which we subsequently optimized using the finite-volume method combined with least-squares analysis. The heat conductivity increased as the temperature increased until the feed began to expand into foam, at which point the conductivity dropped. It began to increase again as the foam turned into a bubble-free glass melt. We discuss the implications of this behavior for the mathematical modeling of the cold cap.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Demonstration test results of organic materials' volumetric reduction using bio-ethanol, thermal decomposition and burning

To discover technologies that can be utilized for decontamination work and verify their effects, economic feasibility, safety, and other factors, the Ministry of the Environment launched the 'FY2011 Decontamination Technology Demonstrations Project' to publicly solicit decontamination technologies that would be verified in demonstration tests and adopted 22 candidates. JAEA was commissioned by the Ministry of the Environment to provide technical assistance related to these demonstrations. This paper describes the volume reduction due to bio-ethanol, thermal decomposition and burning of organic materials in this report. The purpose of this study is that to evaluate a technique that can be used as biomass energy source, while performing volume reduction of contamination organic matter generated by decontamination. An important point of volume reduction technology of contaminated organic matter, is to evaluate the mass balance in the system. Then, confirming the mass balance of radioactive material and where to stay is important. The things that are common to all technologies, are ensuring that the radioactive cesium is not released as exhaust gas, etc.. In addition, it evaluates the cost balance and energy balance in order to understand the applicability to the decontamination of volume reduction technology. The radioactive cesium remains in the carbides when organic materials are carbonized, and radioactive cesium does not transfer to bio-ethanol when organic materials are processed for bio-ethanol production. While plant operating costs are greater if radioactive materials need to be treated, if income is expected by business such as power generation, depreciation may be calculated over approximately 15 years. (authors)

09 BIOMASS FUELS↗

DOE OSTI2020

Influences of Mg Ions and Al Ions on Deposition Behavior of Supersaturated Silicic Acid - 20261

Silicic acid can change into various species such as deposit, colloidal, and soluble form under certain conditions: for example, gradual pH changes around geological disposal repositories. In particular, silicic acid deposits narrow groundwater flow paths, thereby restricting the flow of groundwater. Such effects may contribute to a delay in radionuclide migration. Previous studies have reported that silicic acid supersaturated in sodium and calcium ions can narrow the flow paths. This study examined the effect of magnesium (Mg) and aluminum (Al) ions on the deposition of supersaturated silicic acid on the solid phase. The deposition behavior of supersaturated silicic acid on the solid phase was investigated in a batch system while changing the initial supersaturation concentration, the coexisting ion concentration, and the amount of added solid phase. In the presence of Mg ions, silicic acid precipitation increased with increasing Mg ion concentration due to the influence of the electrolyte, and crosslinking reactions. The coexistence of Al ions significantly suppressed silicic acid deposition due to the formation of a covering on the solid surface during Al ion hydrolysis under conditions of high Al concentration (1.4 mM). On the basis of these experimental results, the apparent deposition rate constant of silicic acid was estimated to be in the range from 10{sup -11} to 10{sup -10} m/s. The Damkoehler number (the dimensionless number expressed by the ratio of the characteristic time of mass transfer and the chemical reaction constant) was sufficient to cause the clogging of the host rock by deposition. This suggests that supersaturated silicic acid deposition, regardless of the presence of Mg ions (and Al ions), contributes to improving barrier performance against radionuclide migration in the host rock. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2020

Middlesex South FUSRAP Site: Collaboration Towards Beneficial Reuse - 20338

The US Department of Energy (DOE) Office of Legacy Management (LM) manages DoE's post-closure responsibilities and ensures the future protection of human health and the environment with respect to sites that have no continuing DOE mission after undergoing remediation. LM's beneficial reuse program promotes the LM strategic goal to sustainably manage and optimize use of public lands. The beneficial reuse program aims to repurpose former contaminated sites to restore the environment, protect the public health, revitalize communities, and spur economic growth. Benefits from the reuse of a site may increase the local tax base, facilitate job growth, utilize existing infrastructure, and enhance or protect natural resources. Beneficial reuse also promotes protectiveness by ensuring activities are compatible with long-term maintenance and protection of public health and the environment, as well as by retaining good stewardship of natural resources. LM actively participates in promoting the economic development vision of the surrounding communities by collaborating with local communities to promote regional or municipal initiatives. The Borough of Middlesex, New Jersey, has prepared the Lincoln Boulevard Redevelopment Plan, which will reinvent a once-viable downtown and enhance the quality of life for the community. The Middlesex South, New Jersey, Formerly Utilized Sites Remedial Action Program (FUSRAP) site lies within the boundaries of this redevelopment area. In support of this development plan, the Borough is interested in acquiring the site for its Department of Public Works and to increase street access in the future commercial district to be built near adjacent properties. The opportunity to put the FUSRAP site into productive use aligns with LM's mission and strategic goals. In support of beneficial reuse activities, DOE can dispose of excess real property using several mechanisms. The two disposal options applicable to the Middlesex south site include (1) utilizing the US General Services Administration (GSA) or (2) using the Title 10 Code of Federal Regulations Section 770, 'Transfer of Real Property at Defense Nuclear Facilities for Economic Development' (known as a '770 transfer') process. Using the 770 transfer requires economic development as the primary driver, and a specific redevelopment proposal must be submitted. If there is no interest in specific economic development, the GSA option becomes the default mechanism for disposal of the property. In the case of the Middlesex south site, the 770 transfer process is being utilized and the Borough has submitted its economic development proposal to LM. Although LM is encouraged by the opportunity to put the site into productive use, the Middlesex south site is currently on the US Environmental Protection Agency (EPA) National Priorities List and remediation is being performed by the US Army Corp of Engineers (USACE) under the Comprehensive Environmental Response, Compensation, and Liability Act (CERCLA). Consequently, any property transfer must meet the requirements under CERCLA Section 120(h), 'Property Transferred by Federal Agencies.' As the groundwater remedy will not be in place for several years, approval would be required from the US EPA administrator and the governor of the state of New Jersey to perform an early transfer of the site (before all response actions have been completed). The time frame for these approvals to occur under the normal process conflicts with the proposed redevelopment schedule; therefore, various options for expedited sale, transfer, or lease of portions of the site to the Borough were evaluated. The subsequent decision on a mutually beneficial path forward was the result of a collaborative effort between LM, USACE, the Borough and its redevelopment team, EPA, and the New Jersey Department of Environmental Protection. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2022

Electrochemical CO2 conversion to formic acid through the Andora Process

Electrochemical utilization or conversion of CO2 can be used to convert waste CO2 into targeted high-value and cost-effective commercial products. Conventional processes for CO2 conversion to fuel sources are challenging and expensive due to their requirement for high temperatures and pressures. Electrochemically, a catalyst can be used at a fixed applied potential to reduce CO2 to form a desired product with less competition at modest operating conditions. Formic acid (FA) has recently become a product of interest for CO2 conversion due to its potential for hydrogen storage and fuel cell applications. Electrochemically, FA is produced through a direct two-electron transfer process involving CO2 with a proton source, requiring less energy input and fewer reaction steps than traditional processes. However, there remain significant obstacles for the broader-scale implementation of CO2 on the market, including competition with unwanted CO and H, the presence of molecular oxygen, and stability of the electrocatalyst. In order to overcome some of these challenges, a new continuous flow Andora Process was developed consisting of two separate cells to decouple electrochemical reduction of the charge carrier with the FA production via an engineered catalyst. Recent experimental results show that with appropriate design changes and operating conditions to the flow system, FA production above 500 mM can be achieved along with efficiencies above 80%. TEA and LCA assessments of the Andora Process show a potential for the reduction in the GWP potential and cost saving compared to the current comparative formic acid production process.

60 APPLIED LIFE SCIENCES↗

NASA NTRS2012

Thermosyphon Flooding Limits in Reduced Gravity Environments

Fission Power Systems have long been recognized as potential multi-kilowatt power solutions for lunar, Martian, and extended planetary surface missions. Current heat rejection technology associated with fission surface power systems has focused on titanium water thermosyphons embedded in carbon composite radiator panels. The thermosyphons, or wickless heat pipes, are used as a redundant and efficient way to spread the waste heat from the power conversion unit(s) over the radiator surface area where it can be rejected to space. It is well known that thermosyphon performance is reliant on gravitational forces to keep the evaporator wetted with the working fluid. One of the performance limits that can be encountered, if not understood, is the phenomenon of condenser flooding, otherwise known as evaporator dry out. This occurs when the gravity forces acting on the condensed fluid cannot overcome the shear forces created by the vapor escaping the evaporator throat. When this occurs, the heat transfer process is stalled and may not re-stabilize to effective levels without corrective control actions. The flooding limit in earth's gravity environment is well understood as experimentation is readily accessible, but when the environment and gravity change relative to other planetary bodies, experimentation becomes difficult. An innovative experiment was designed and flown on a parabolic flight campaign to achieve the Reduced Gravity Environments (RGE) needed to obtain empirical data for analysis. The test data is compared to current correlation models for validation and accuracy.

Gibson, Marc A.↗

DOE OSTI2012

Ceramic HEPA Filter Program

Potential benefits of ceramic filters in nuclear facilities: (1) Short term benefit for DOE, NRC, and industry - (a) CalPoly HTTU provides unique testing capability to answer questions for DOE - High temperature testing of materials, components, filter, (b) Several DNFSB correspondences and presentations by DNFSB members have highlighted the need for HEPA filter R and D - DNFSB Recommendation 2009-2 highlighted a nuclear facility response to an evaluation basis earthquake followed by a fire (aka shake-n-bake) and CalPoly has capability for a shake-n-bake test; (2) Intermediate term benefit for DOE and industry - (a) Filtration for specialty applications, e.g., explosive applications at Nevada, (b) Spin-off technologies applicable to other commercial industries; and (3) Long term benefit for DOE, NRC, and industry - (a) Across industry, strong desire for better performance filter, (b) Engineering solution to safety problem will improve facility safety and decrease dependence on associated support systems, (c) Large potential life-cycle cost savings, and (d) Facilitates development and deployment of LLNL process innovations to allow continuous ventilation system operation during a fire.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2018

Updating the Dry Transfer System - 18110

The Dry Transfer System (DTS) was examined for its ability to be redesigned in order to meet needs associated with repackaging used/spent nuclear fuel (UNF/SNF) from existing storage cask systems into alternative systems, while also incorporating design advances based on some lessons learned from Orano's dry UNF handling facility (T0) located at the La Hague recycling plant. In this redesign, the DTS is envisioned to provide some flexibility through the ability to perform repackaging activities from multiple differently designed cask systems, including those with canisters that will require cutting and welding activities, and potentially with waste packages designed for disposal. The redesigned DTS is also intended to provide some operational flexibility by providing lag storage and include a means for examining UNF/SNF during repackaging, using some features implemented at the T0 facility at La Hague. This paper provides a summary of: the original DTS design, which was evaluated by the NRC and portions of which were cold-tested at Idaho National Lab; the lag storage system designed for the DTS, which is able to flexibly handle different fuel assembly designs while providing structural support for design basis events (e.g., seismic); the incorporation of lessons learned from the La Hague T0 facility into the DTS design to facilitate dry handling of UNF/SNF; and identification of other challenges towards designing a complete system. A revised DTS is envisioned to provide an important tool for the future management of UNF/SNF in preparation for transportation, re-storage, re-transportation, and/or disposal and also provides a means for repackaging UNF/SNF in case recovery from a cask/canister system is necessary (e.g., due to extended storage or a transportation event). (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2016

In-Situ Gamma-Ray Assay of the 235-F Plutonium Fuel Form Facility at the Savannah River Site - 16293

The Plutonium Fuel Form (PuFF) Facility is located in Building 235-F near the geographic center of the Savannah River Site. Between 1978 and 1984, the facility was used to produce approximately 165 kilograms of iridium-encapsulated Pu-238 spheres and pellets for use as radioisotope thermal generators, primarily for the space program. The facility is divided between two cell lines, the east cell line used to process powdered Pu-238 oxide raw material into fuel forms and the west cell line used to encapsulate the fuel forms in iridium. Scoping in-situ gamma-ray assays were performed in the PuFF Facility in 2006 and estimated that hundreds of grams of Pu-238 holdup were within the facility. Using this holdup estimate as a source term, SRS has performed a risk analysis that indicated a seismic event that induces a full-facility fire in 235-F could lead to a 28,800 rem dose to a co-located worker. Based on this risk assessment, SRS is taking steps to decontaminate the facility. One of the first steps taken has been to improve upon the quality of the in-situ gamma-ray assay data. Carts and collimators were specially designed to survey the equipment in the PuFF Facility. The cell interiors were assayed along with the furnaces and storage coolers that protrude beneath the cells. While the previous scoping work consisted of 32 measurements, the current series of measurements included nearly 400 measurements using both high-purity germanium and lanthanum bromide detectors. Data analysis for the current set of measurements was conducted with greater rigor as well. MCNP5 was used to evaluate a variety of possible physical distributions for the Pu-238 source term and estimate cross-talk between neighboring cells. Data analysis was performed using three gamma-rays emitted by Pu-238 (99.85 keV, 152.7 keV, and 766.4 keV) providing three independent estimates of the mass of Pu-238 holdup in each of the cells. This also allowed the application of matrix correction factors to adjust gamma-ray attenuation. The weighted mean of these three results was used as the best estimate of Pu-238 holdup in the PuFF facility. This work lowered the estimate of holdup in the PuFF facility by approximately 100 grams compared to the previous estimate, a 0.55's difference. The uncertainty in the Pu-238 holdup was also reduced substantially relative to the 2006 scoping assay. Further radiological measurements are planned for the near future including in-situ gamma-ray assays of wing cabinets in the east cell line maintenance area, the transfer tube between the two cell lines, and some of the furnaces and storage coolers. A germanium gamma imager, the GeGI, will also be used to map out the distribution of the Pu-238 source term in the PuFF Facility. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2021

Green hydrogen from microalgal liquefaction byproducts with ammonia recovery and effluent recycle for developing circular processes

Hydrothermal liquefaction is a promising technology for microalgae-based biofuel production. However, hydrothermal liquefaction’s aqueous wastes have little established reuse, and contain significant fractions of toxic ammoniacal nitrogen. Careful reuse of this waste can assure microalgae-based biofuels are produced with less environmental impact and larger energy efficiency. Microbial electrolysis cells were investigated to valorize this waste product by converting the leftover organics into hydrogen and remove ammonia. Waste hydrothermal liquefaction aqueous phase from two microalgal strains, Tetraselmis sp. and Chlorella sp. were used as feedstocks for hydrogen production in microbial electrolysis cells. Chlorella and Tetraselmis aqueous phase-fed microbial electrolysis cells reach an average current density of 5.1 ± 0.19 A/m 2 and 3.8 ± 0.08 A/m 2 . Compound removal rates and mass removal percentages were also investigated for each feedstock. Additionally, acetic acid, propionic acid, ethanol, and glycerol were effectively removed from the aqueous byproduct. Further, microbial electrolysis cells separated up to 34.3% of ammoniacal nitrogen present in the aqueous phase. Charge transfer analysis indicated that proton transfer, not ammonium transfer, contributed to the majority of the hydrogen production in the cathode. Finally, the microbial electrolysis cell effluent was reused to grow the same microalgal strains, leading to the development of a circular biofuel production system. Microalgae regrowth studies using microbial electrolysis cell effluent showed nearly complete removal of total organic carbon, but significantly less removal of total nitrogen. Tetraselmis sp. growth occurred with the Tetraselmis-derived MEC effluent, however, the control medium without effluent produced the most growth. These findings support the possibility of a circular biofuel framework using MECs, but additional constraints, including the removal of inorganic contaminants, are necessary to realize the circular processes.

09 BIOMASS FUELS↗

DOE OSTI2020

Construction-Scale Concrete Additive Manufacturing and its Application in Infrastructure Energy Storage

Construction is filled with labor intensive, hazardous, and often wasteful processes. It is also an enormous industry, so improvements in efficiency could have a tremendous economic impact. Construction-scale additive manufacturing is one path toward achieving those improvements. In this paper, a construction-scale additive manufacturing system, called Sky-BAAM, is presented. In addition to possibly leading to more energy-efficient construction practices, leveraging additive manufacturing in construction opens the solution space to more energy efficient building design. One such design, the EMPOWER wall, is also presented in this paper. The exterior of the wall is shaped to maximize heat transfer, while acting as form work for an internal energy-storage system. This allows energy to be stored in the wall during off-peak times and retrieved during peak periods.

Atkins, Celeste↗

DOE OSTI2018

Handling and Treatment of Sodium-Potassium Alloy (NaK) after the Loss of Key Personnel – 19002

ABSTRACT In September 2010, during cleanup and removal efforts associated with a glovebox containing a sodium-potassium alloy (NaK) cooling system, a NaK reaction event occurred. Near the end of the evolution, which was at a Materials and Fuels Complex (MFC) research facility at the Idaho National Laboratory, a 2 to 3-ounce sample of NaK was being transferred from a metal can to a polyethylene bottle so it could be sent to the disposal outlet for verification analysis. During the transfer, a reaction of the NaK with ambient air was observed in both the metal can and sample container. The potential for a reaction was identified during the planning of this activity and mitigating steps were included in the procedures. In response, the two containers were flooded with argon, closed, and observed overnight. No additional reaction was noted. The sample container and metal can were packaged into a 10-gallon drum and transferred to a permitted storage location pending disposal. While the other containers generated from the deactivation and decommissioning activity were sent off-site for disposal, the 10-gal drum remained due to concerns by a staff specialist that the material could contain potassium superoxide (KO2) as a result of the reaction event. The intent at that time was to treat the NaK in a Resource Conservation and Recovery Act (RCRA)-permitted treatment facility at MFC, instead of sending it off-site for disposal. The container was labeled, inspected, and managed as a hazardous waste. Due to the complexities associated with safely handling and treating NaK and KO2, the container remained in storage. Treatment and disposal of the NaK and KO2 container was revisited in 2016, when researchers and chemists were consulted regarding the potential for superoxide formation and the best means to safely store and treat the container. The facility came to realize that due to the retirements of key personnel, it needed to provide current employees operational experience with the handling and treatment of NaK. An outside company was identified and contracted to provide training and consulting services. Several Battelle Energy Alliance, Inc. (BEA) personnel then attended an alkali metals safety training class. The training course provided participants with classroom and hands–on instruction associated with: • Hazards associated with handling and using sodium and NaK • Proper personal protection equipment, spill control techniques, and first aid • Common design approaches for buildings, systems, and equipment used to contain sodium and NaK • What to expect in the event of a water reaction and how to respond • How to properly prepare for a fire and contain/extinguish small metal fires • A hands-on demonstration of NaK reaction and controls. Following the training, a procedure was developed to open the container, and inspect and treat the NaK. In June 2017, facility operations personnel successfully completed the inspection and treatment of the NaK drum, eliminating the legacy liability.

99 GENERAL AND MISCELLANEOUS↗

DOE OSTI2018

The Effect of Environmental Relative Humidity on Carbonation and Oxidation in a Cementitious Waste Form - 18448

Cementitious material has been developed and used for the nuclear waste disposal. Cast Stone, a type of cementitious waste form, is considered for solidification and immobilization of part of low activity radioactive waste (LAW) at DOE Hanford Site in Richland, WA. During its life cycle, the waste form, which is produced from Portland cement, fly ash, blast furnace slag and liquid waste, is subject to reaction with carbon dioxide and oxygen, both in gaseous and dissolved form. The reactions may alter the physical and chemical properties of the waste form and thus change its retention ability for the radionuclides. Therefore, understanding the rate and the impact of oxidation and carbonation in the material is important for projecting the long-term performance of Cast Stone. However, the rate of carbonation and oxidation in Cast Stone closely depends on the moisture content in the material, which varies largely with the environmental relative humidity (RH). In this study, experiments are carried out to study the effect of environmental relative humidity on the carbonation and oxidation rate as well as the leaching of the constituents from Cast Stone. Cast Stone samples doped with Cr as a reaction indicator are aged for 16 to 32 weeks under N{sub 2}, air, and 2% CO{sub 2} (in nitrogen) environments with various relative humidities (15%, 40%, 68%, 100%). After aging, samples were tested for the pH-dependent leaching (EPA Method 1313) and mass transfer rate under diffusion-controlled leaching (EPA Method 1315) of constituents. The progress of the carbonation was measured for each condition to determine the rate of carbonation front ingress. The results show that environmental relative humidity strongly influences carbonation and oxidation in Cast Stone; however, the impact is different for the rate of reaction and for the extent of reactions. The former refers to the rate at which the reaction front ingresses, while the latter refers to the fraction of the material reacted. For both carbonation and oxidation, the largest impact of the reactions at the exposure surface is observed at intermediate relative humidity (68%). However, for carbonation, the reaction front evolves more rapidly under drier conditions, with the highest rate observed at 15% RH. As a result, carbonation and oxidation have different degree of impact on the leaching behavior of Cast Stone samples aged under various relative humidities. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2015

Quick-start of full-scale anaerobic digestion (AD) using aeration

Highlights: • A fast, and original, start up procedure for anaerobic digestors has been applied at full scale. • The development of a methanogenic culture has been documented using fluorescent in situ hybridization. • The technique can be widely applied. - Abstract: A conventional 1300 m{sup 3} continuously stirred anaerobic tank reactor at the city of Boden, north Sweden, which was receiving a feed of both sewage sludge and food waste, was put out of operation due to the build-up of a float phase. The reactor was emptied and cleaned. At start-up there was no methanogenic sludge available, so an unconventional start-up procedure was applied: The reactor was rapidly (8 days with 1200 kg of total solids (TS) added daily) filled with thickened, and slightly acidic sewage sludge, showing only slight methane generation, which was subsequently heated to 55 °C. Then compressed air was blown into the digester and within a month a fully functional methanogenic culture was established. The transfer from acidogenic to methanogenic conditions happened in about one week. As a start-up technique this is fast and cost efficient, it only requires the access of a compressor, electricity and a source of air. In total, about 16 tonnes of oxygen were used. It is proposed that this method may also be used as an operational amendment technique, should a reactor tend to acidify.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2012

Deep Bed Adsorption Testing using Silver-Functionalized Aerogel

Nuclear fission results in the production of fission products and activation products, some of which tend to be volatile during used fuel reprocessing and evolve in gaseous species into the reprocessing facility off-gas systems. Analyses have shown that I129, due to its radioactivity, high potential mobility in the environment, and high longevity (half life of 15.7 million years), can require control efficiencies of up to 1,000x or higher to meet regulatory emission limits. Two Aerogel sorption tests that have been performed this fiscal year. The maximum iodine decontamination factor (DF) was measured to be over 10,000, above the 1,000-10,000 target DF range. The mass transfer zone may be as short as 0.5 inches under the sorption conditions of the first test. Only a small fraction of the iodine sorbed on Bed 1 was desorbed during the purge periods. The silver-functionalized Aerogel appears to have potential to be a very effective and efficient iodine sorbent.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2018

Ediesel: Diesel Additive production from ethanol and bio-diesel coproducts

This project has focused on supporting and expanding the U.S. ethanol industry by developing new conversion routes and products from ethanol and the byproducts made in ethanol fermentation. The work is relevant to the DOE program goals of developing high-margin chemical products in the biorefinery to economically support large-scale biofuel production. The higher alcohols from condensation of ethanol, alkylated amine compounds made by electrocatalytic alkyation, and fusel alcohols produced by modified fermentation microorganisms are all existing or potentially large-scale commodity or specialty chemicals with well-defined uses in industry. The formation of higher alcohols from ethanol in the condensed phase developed several catalysts, first in stirred batch autoclave reactors and then in a continuous flow reactor system, to achieve significant yields of n-butanol and higher alcohols. The best selectivity to higher alcohols exceeded 80% of theoretical at ethanol conversions of 30-40%. From the laboratory experiments and analysis of the phase equilibria of the species involved, a process concept was generated and simulated in AspenPlus to determine the specifications of the various equipment involved in the process. Results show that for the conversion and selectivity described above, the required n-butanol selling price of ~$1.60/kg is in the range of current n-butanol selling price in the marketplace. Several additional permutations of the process, along with evaluation of higher conversion and selectivities to desired alcohol products, showed that the production of n-butanol from ethanol should be competitive in the marketplace as the science and engineering behind the process improves with continued development. A second aspect of the project focused on producing fusel alcohols in increased quantities during ethanol fermentation. Fusel alcohols, which are composed primarily of isoamyl alcohol and minor quantities of C3-C6 alcohols, have potential as higher value feed stocks for specialty chemical production. Several strains of yeast were evaluated for fusel alcohol production, and the most efficient process for separating and purifying fusel alcohols was developed from both experiments and simulation. Finally, model fusel alcohol mixtures were subjected to condensation reactions with ethanol to prepare higher alcohols that again have potential for specialty chemical or solvent applications. In this preliminary work, measurable quantities of several species were observed, including some species that were previously unknown or uncharacterized in the literature. The third aspect of the project involved the electrocatalytic alkylation of amines with alcohols to form alkyl amines. Ethanol has been demonstrated to serve as an effective ethyl group transfer agent to the nitrogen centers of amines, a reaction with only water as a byproduct. Mild reaction conditions (60 °C, aqueous solution) are enabled by the novel use of simple, undivided electrochemical cell reactors that include long-lived, low cost catalytic electrodes. Direct polyalkylation of ammonia and isolation of the resulting triethylamine product was readily achieved in high yield. Though classical high temperature and pressure industrial scale alkylations reactions will likely continue to be used for production of simple product such as triethylamine, this approach has opened the door to the low cost, low waste use of ethanol and related primary and secondary alcohols to alkylate more delicate amines that were heretofore difficult to synthesize.

02 PETROLEUM↗

DOE OSTI2015

Automation of environmental compliance data acquisition and management - 15267

Regulatory sampling for environmental compliance at the Savannah River Site (SRS), Aiken, South Carolina employs several different types of sampling techniques at various sampling frequencies. These sampling events result in the collection of large quantities of data and generate substantial data-related documents. The use of paper documents resulted in the need for manual input of data collected in the field and distribution of documents from one group to the next. To efficiently and effectively manage the extensive amounts of data and documents, elements of the sampling process were automated using hand-held field tablets and an electronic application. The tablets allow for easier distribution of sampling documents, and the application allows for digital transfer of sampling information and collected field data. The transition to automated data acquisition and management has resulted in a more efficient and reliable manner for conducting business at SRS. This system benefits numerous organizations at SRS by utilizing a centralized database for efficient management of all environmental data collected. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2019

Handling and Treatment of Sodium-Potassium Alloy (NaK) after the Loss of Key Personnel - 19002

In September 2010, during cleanup and removal efforts associated with a glovebox containing a sodium-potassium alloy (NaK) cooling system, a NaK reaction event occurred. Near the end of the evolution, which was at a Materials and Fuels Complex (MFC) research facility at the Idaho National Laboratory, a 2 to 3-ounce sample of NaK was being transferred from a metal can to a polyethylene bottle so it could be sent to the disposal outlet for verification analysis. During the transfer, a reaction of the NaK with ambient air was observed in both the metal can and sample container. The potential for a reaction was identified during the planning of this activity and mitigating steps were included in the procedures. In response, the two containers were flooded with argon, closed, and observed overnight. No additional reaction was noted. The sample container and metal can were packaged into a 10-gallon drum and transferred to a permitted storage location pending disposal. While the other containers generated from the deactivation and decommissioning activity were sent off-site for disposal, the 10-gal drum remained due to concerns by a staff specialist that the material could contain potassium superoxide (KO{sub 2}) as a result of the reaction event. The intent at that time was to treat the NaK in a Resource Conservation and Recovery Act (RCRA)-permitted treatment facility at MFC, instead of sending it off-site for disposal. The container was labeled, inspected, and managed as a hazardous waste. Due to the complexities associated with safely handling and treating NaK and KO{sub 2}, the container remained in storage. Treatment and disposal of the NaK and KO{sub 2} container was revisited in 2016, when researchers and chemists were consulted regarding the potential for superoxide formation and the best means to safely store and treat the container. The facility came to realize that due to the retirements of key personnel, it needed to provide current employees operational experience with the handling and treatment of NaK. An outside company was identified and contracted to provide training and consulting services. Several Battelle Energy Alliance, Inc. (BEA) personnel then attended an alkali metals safety training class. The training course provided participants with classroom and hands-on instruction associated with: - Hazards associated with handling and using sodium and NaK; - Proper personal protection equipment, spill control techniques, and first aid; - Common design approaches for buildings, systems, and equipment used to contain sodium and NaK; - What to expect in the event of a water reaction and how to respond; - How to properly prepare for a fire and contain/extinguish small metal fires; - A hands-on demonstration of NaK reaction and controls. Following the training, a procedure was developed to open the container, and inspect and treat the NaK. In June 2017, facility operations personnel successfully completed the inspection and treatment of the NaK drum, eliminating the legacy liability. (authors)

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗