12 research outputs found
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Removal of Solids From Highly Enriched Uranium Solutions Using the H-Canyon Centrifuge
Prior to the dissolution of Pu-containing materials in HB-Line, highly enriched uranium (HEU) solutions stored in Tanks 11.1 and 12.2 of H-Canyon must be transferred to provide storage space. The proposed plan is to centrifuge the solutions to remove solids which may present downstream criticality concerns or cause operational problems with the 1st Cycle solvent extraction due to the formation of stable emulsions. An evaluation of the efficiency of the H-Canyon centrifuge concluded that a sufficient amount (> 90%) of the solids in the Tank 11.1 and 12.2 solutions will be removed to prevent any problems. We based this conclusion on the particle size distribution of the solids isolated from samples of the solutions and the calculation of particle settling times in the centrifuge. The particle size distributions were calculated from images generated by scanning electron microscopy (SEM). The mean particle diameters for the distributions were 1-3 {micro}m. A significant fraction (30-50%) of the particles had diameters which were < 1 {micro}m; however, the mass of these solids is insignificant (< 1% of the total solids mass) when compared to particles with larger diameters. It is also probable that the number of submicron particles was overestimated by the software used to generate the particle distribution due to the morphology of the filter paper used to isolate the solids. The settling times calculated for the H-Canyon centrifuge showed that particles with diameters less than 1 to 0.5 {micro}m will not have sufficient time to settle. For this reason, we recommend the use of a gelatin strike to coagulate the submicron particles and facilitate their removal from the solution; although we have no experimental basis to estimate the level of improvement. Incomplete removal of particles with diameters < 1 {micro}m should not cause problems during purification of the HEU in the 1st Cycle solvent extraction. Particles with diameters > 1 {micro}m account for > 99% of the solid mass and will be efficiently removed by the centrifuge; therefore, the formation of emulsions during solvent extraction operations is not an issue. Under the current processing plan, the solutions from Tanks 11.1 and 12.2 will be transferred to the enriched uranium storage (EUS) tank following centrifugation. The solution from Tanks 11.1 and 12.2 may remain in the EUS tank for an extended time prior to purification. The effects of extended storage on the solution were not evaluated as part of this study
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SODIUM ALUMINOSILICATE FOULING AND CLEANING OF DECONTAMINATED SALT SOLUTION COALESCERS
During initial non-radioactive operations at the Modular Caustic Side Solvent Extraction Unit (MCU), the pressure drop across the decontaminated salt solution coalescer reached {approx}10 psi while processing {approx}1250 gallons of salt solution, indicating possible fouling or plugging of the coalescer. An analysis of the feed solution and the 'plugged coalescer' concluded that the plugging was due to sodium aluminosilicate solids. MCU personnel requested Savannah River National Laboratory (SRNL) to investigate the formation of the sodium aluminosilicate solids (NAS) and the impact of the solids on the decontaminated salt solution coalescer. Researchers performed developmental testing of the cleaning protocols with a bench-scale coalescer container 1-inch long segments of a new coalescer element fouled using simulant solution. In addition, the authors obtained a 'plugged' Decontaminated Salt Solution coalescer from non-radioactive testing in the MCU and cleaned it according to the proposed cleaning procedure. Conclusions from this testing include the following: (1) Testing with the bench-scale coalescer showed an increase in pressure drop from solid particles, but the increase was not as large as observed at MCU. (2) Cleaning the bench-scale coalescer with nitric acid reduced the pressure drop and removed a large amount of solid particles (11 g of bayerite if all aluminum is present in that form or 23 g of sodium aluminosilicate if all silicon is present in that form). (3) Based on analysis of the cleaning solutions from bench-scale test, the 'dirt capacity' of a 40 inch coalescer for the NAS solids tested is calculated as 450-950 grams. (4) Cleaning the full-scale coalescer with nitric acid reduced the pressure drop and removed a large amount of solid particles (60 g of aluminum and 5 g of silicon). (5) Piping holdup in the full-scale coalescer system caused the pH to differ from the target value. Comparable hold-up in the facility could lead to less effective cleaning and precipitation of bayerite solid particles. (6) Based on analysis of the cleaning solutions from the full-scale test, the 'dirt capacity' of a 40 inch coalescer for these NAS solids was calculated to be 40-170 grams
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ANALYSIS OF SOLVENT RECOVERED FROM WRIGHT INDUSTRIES, INCORPORATED TESTING
Washington Savannah River Company (WSRC) began designing and building a Modular Caustic Side Solvent Extraction (CSSX) Unit (MCU) at the Savannah River Site (SRS) to process liquid waste for an interim period. The MCU Project Team conducted testing of the contactors, coalescers, and decanters at Wright Industries, Incorporated (WII) in Nashville, Tennessee. That testing used MCU solvent and simulated SRS dissolved salt. Because of the value of the solvent, the MCU Project wishes to recover it for use in the MCU process in the H-Tank Farm. Following testing, WII recovered approximately 62 gallons of solvent (with entrained aqueous) and shipped it to SRS. The solvent arrived in two stainless steel drums. The MCU Project requested SRNL to analyze the solvent to determine whether it is suitable for use in the MCU Process. SRNL analyzed the solvent for Isopar{reg_sign} L by Gas Chromatography--Mass Spectroscopy (GC-MS), for Modifier and BOBCalixC6 by High Pressure Liquid Chromatography (HPLC), and for Isopar{reg_sign} L-to-Modifier ratio by Fourier-Transform Infrared (FTIR) spectroscopy. They also measured the solvent density gravimetrically and used that measurement to calculate the Isopar{reg_sign} L and Modifier concentration. The conclusions from this work are: (1) The constituents of the used WII solvent are collectively low in Isopar{reg_sign} L, most likely due to evaporation. This can be easily corrected through the addition of Isopar{reg_sign} L. (2) Compared to a sample of the WII Partial Solvent (without BOBCalixC6) archived before transfer to WII, the Reworked WII Solvent showed a significant improvement (i.e., nearly doubling) in the dispersion numbers for tests with simulated salt solution and with strip acid. Hence, the presence of the plasticizer impurity has no detrimental impact on phase separation. While there are no previous dispersion tests using the exact same materials, the results seem to indicate that the washing of the solvent gives a dispersion benefit. (3) WII Solvent that underwent a cleaning cycle provides an acceptable set of cesium distribution (i.e., D) values when used in a standard Extraction, Scrub, and Strip (ESS) test
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Reactivity of Resorcinol Formaldehyde Resin with Nitric Acid
Solid-state infrared spectroscopy, differential scanning calorimetry, and elemental analysis have been used to evaluate the reactivity of resorcinol formaldehyde resin with nitric acid and characterize the solid product. Two distinct reactions were identified within the temperature range 25-55 C. The first reaction is primarily associated with resin nitration, while the second involves bulk oxidation and degradation of the polymer network leading to dissolution and off-gassing. The threshold conditions promoting reaction have been identified. Reaction was confirmed with nitric acid concentrations as low as 3 M at 25 C applied temperature and 0.625 M at 66 C. Although a nitrated resin product can be isolated under appropriate experimental conditions, calorimetry testing indicates no significant hazard associated with handling the dry material
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IN-SITU MONITORING OF CORROSION DURING A LABORATORY SIMULATION OF OXALIC ACID CHEMICAL CLEANING
The Savannah River Site (SRS) will disperse or dissolve precipitated metal oxides as part of radioactive waste tank closure operations. Previously SRS used oxalic acid to accomplish this task. To better understand the conditions of oxalic acid cleaning of the carbon steel waste tanks, laboratory simulations of the process were conducted to determine the corrosion rate of carbon steel and the generation of gases such as hydrogen and carbon dioxide. Open circuit potential measurements, linear polarization measurements, and coupon immersion tests were performed in-situ to determine the corrosion behavior of carbon steel during the demonstration. Vapor samples were analyzed continuously to determine the constituents of the phase. The combined results from these measurements indicated that in aerated environments, such as the tank, that the corrosion rates are manageable for short contact times and will facilitate prediction and control of the hydrogen generation rate during operations
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INVESTIGATING HYDROGEN GENERATION AND CORROSION IN THE TREATMENT TANK AND THE POTENTIAL FORMATION OF A FLOATING LAYER IN NEUTRALIZATION TANK DURING WASTE TANK HEEL CHEMICAL CLEANING
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REMOVING SLUDGE HEELS FROM SAVANNAH RIVER SITE WASTE TANKS BY OXALIC ACID DISSOLUTION
The Savannah River Site (SRS) will remove sludge as part of waste tank closure operations. Typically the bulk sludge is removed by mixing it with supernate to produce a slurry, and transporting the slurry to a downstream tank for processing. Experience shows that a residual heel may remain in the tank that cannot be removed by this conventional technique. In the past, SRS used oxalic acid solutions to disperse or dissolve the sludge heel to complete the waste removal. To better understand the actual conditions of oxalic acid cleaning of waste from carbon steel tanks, the authors developed and conducted an experimental program to determine its effectiveness in dissolving sludge, the hydrogen generation rate, the generation rate of other gases, the carbon steel corrosion rate, the impact of mixing on chemical cleaning, the impact of temperature, and the types of precipitates formed during the neutralization process. The test samples included actual SRS sludge and simulated SRS sludge. The authors performed the simulated waste tests at 25, 50, and 75 C by adding 8 wt % oxalic acid to the sludge over seven days. They conducted the actual waste tests at 50 and 75 C by adding 8 wt % oxalic acid to the sludge as a single batch. Following the testing, SRS conducted chemical cleaning with oxalic acid in two waste tanks. In Tank 5F, the oxalic acid (8 wt %) addition occurred over seven days, followed by inhibited water to ensure the tank contained enough liquid to operate the mixer pumps. The tank temperature during oxalic acid addition and dissolution was approximately 45 C. The authors analyzed samples from the chemical cleaning process and compared it with test data. The conclusions from the work are: (1) Oxalic acid addition proved effective in dissolving sludge heels in the simulant demonstration, the actual waste demonstration, and in SRS Tank 5F. (2) The oxalic acid dissolved {approx} 100% of the uranium, {approx} 100% of the iron, and {approx} 40% of the manganese during a single contact in the simulant demonstration. (The iron dissolution may be high due to corrosion of carbon steel coupons.) (3) The oxalic acid dissolved {approx} 80% of the uranium, {approx} 70% of the iron, {approx} 50% of the manganese, and {approx} 90% of the aluminum in the actual waste demonstration for a single contact. (4) The oxalic acid dissolved {approx} 100% of the uranium, {approx} 15% of the iron, {approx} 40% of the manganese, and {approx} 80% of the aluminum in Tank 5F during the first contact cycle. Except for the iron, these results agree well with the demonstrations. The data suggest that a much larger fraction of the iron in the sludge dissolved, but it re-precipitated with the oxalate added to Tank 5F. (5) The demonstrations produced large volumes (i.e., 2-14 gallons of gas/gallon of oxalic acid) of gas (primarily carbon dioxide) by the reaction of oxalic acid with sludge and carbon steel. (6) The reaction of oxalic acid with carbon steel produced hydrogen in the simulant and actual waste demonstrations. The volume produced varied from 0.00002-0.00100 ft{sup 3} hydrogen/ft{sup 2} carbon steel. The hydrogen production proved higher in unmixed tanks than in mixed tanks
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MEASUREMENT OF ENTRAINED ORGANIC DROPLET SIZES AND TOTAL CONCENTRATION FOR AQUEOUS STREAMS FROM THE CAUSTIC-SIDE SOLVENT EXTRACTION PROCESS
The Modular Caustic-Side Solvent Extraction Unit (MCU) and the Salt Waste Processing Facility will remove radioactive cesium from Savannah River Site supernate wastes using an organic solvent system. Both designs include decanters and coalescers to reduce carryover of organic solvent droplets. Savannah River National Laboratory personnel conducted experimental demonstrations using a series of four 2-cm centrifugal contactors. They also examined organic carryover during operation of a CINC (Costner Industries Nevada Corporation) V-5 contactor under prototypical conditions covering the range of expected MCU operation. This report details the findings from those studies and the implications on design for the MCU
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DETERMINATION OF LIQUID FILM THICKNESS FOLLOWING DRAINING OF CONTACTORS, VESSELS, AND PIPES IN THE MCU PROCESS
The Department of Energy (DOE) identified the caustic side solvent extraction (CSSX) process as the preferred technology to remove cesium from radioactive waste solutions at the Savannah River Site (SRS). As a result, Washington Savannah River Company (WSRC) began designing and building a Modular CSSX Unit (MCU) in the SRS tank farm to process liquid waste for an interim period until the Salt Waste Processing Facility (SWPF) begins operations. Both the solvent and the strip effluent streams could contain high concentrations of cesium which must be removed from the contactors, process tanks, and piping prior to performing contactor maintenance. When these vessels are drained, thin films or drops will remain on the equipment walls. Following draining, the vessels will be flushed with water and drained to remove the flush water. The draining reduces the cesium concentration in the vessels by reducing the volume of cesium-containing material. The flushing, and subsequent draining, reduces the cesium in the vessels by diluting the cesium that remains in the film or drops on the vessel walls. MCU personnel requested that Savannah River National Laboratory (SRNL) researchers conduct a literature search to identify models to calculate the thickness of the liquid films remaining in the contactors, process tanks, and piping following draining of salt solution, solvent, and strip solution. The conclusions from this work are: (1) The predicted film thickness of the strip effluent is 0.010 mm on vertical walls, 0.57 mm on horizontal walls and 0.081 mm in horizontal pipes. (2) The predicted film thickness of the salt solution is 0.015 mm on vertical walls, 0.74 mm on horizontal walls, and 0.106 mm in horizontal pipes. (3) The predicted film thickness of the solvent is 0.022 mm on vertical walls, 0.91 mm on horizontal walls, and 0.13 mm in horizontal pipes. (4) The calculated film volume following draining is: (a) Salt solution receipt tank--1.6 gallons; (b) Salt solution feed tank--1.6 gallons; (c) Decontaminated salt solution hold tank--1.6 gallons; (d) Contactor drain tank--0.40 gallons; (e) Strip effluent hold tank--0.33 gallons; (f) Decontaminated salt solution decanter--0.37 gallons; (g) Strip effluent decanter--0.14 gallons; (h) Solvent hold tank--0.30 gallon; and (i) Corrugated piping between contactors--16-21 mL. (5) After the initial vessel draining, flushing the vessels with 100 gallons of water using a spray nozzle that produces complete vessel coverage and draining the flush water reduces the source term by the following amounts: (i) Salt solution receipt tank--63X; (ii) Salt solution feed tank--63X; (iii) Decontaminated salt solution hold tank--63X; (iv) Contactor drain tank--250X; (v) Strip effluent hold tank--300X; (vi) Decontaminated salt solution decanter--270X; (vii) Strip effluent decanter--710X; (viii) Solvent hold tank--330X. Understand that these estimates of film thickness are based on laboratory testing and fluid mechanics theory. The calculations assume drainage occurs by film flow. Much of the data used to develop the models came from tests with very ''clean'' fluids. Impurities in the fluids and contaminants on the vessels walls could increase liquid holdup. The application of film thickness models and source term reduction calculations should be considered along with operational conditions and H-Tank Farm/Liquid Waste operating experience. These calculations exclude the PVV/HVAC duct work and piping, as well as other areas that area outside the scope of this report
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Aluminum Leaching of ''Archived'' Sludge from Tanks 8F, 11H, and 12H
Aluminum can promote formation or dissolution of networks in hydroxide solid solutions. When present in large amounts it will act as a network former increasing both the viscosity and the surface tension of melts. This translates into poor free flow properties that affect pour rate of glass production in the Defense Waste Processing Facility (DWPF). To mitigate this situation, DWPF operations limit the amount of aluminum contained in sludge. This study investigated the leaching of aluminum compounds from archived sludge samples. The conclusions found boehmite present as the predominant aluminum compound in sludge from two tanks. We did not identify an aluminum compound in sludge from the third tank. We did not detect any amorphous aluminum hydroxide in the samples. The amount of goethite measured 4.2 percentage weight while hematite measured 3.7 percentage weight in Tank 11H sludge. The recommended recipe for removing gibbsite in sludge proved inefficient for digesting boehmite, removing less than 50 per cent of the compound within 48 hours. The recipe did remove boehmite when the test ran for 10 days (i.e., 7 more days than the recommended baseline leaching period). Additions of fluoride and phosphate to Tank 12H archived sludge did not improve the aluminum leaching efficiency of the baseline recipe