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Anion exchange separation of plutonium from various solutions stored at PFP

Description: Nitrate anion exchange has been demonstrated to effectively separate plutonium from other metals in solution. Specific PFP solutions types will be tested to determine if they are suitable candidates for anion exchange. Reillex HPQ resin is used to separate Pu(IV) from nitric acid solutions.
Date: February 26, 1996
Creator: Jones, S.A.
Partner: UNT Libraries Government Documents Department

Chloride content of dissolver solution from Rocky Flats scrub alloy ninth and tenth campaigns following head end treatment

Description: F-Canyon continues to obtain excellent chloride removal from Rocky Flats scrub alloy (RFSA) dissolver solution during head end treatment. One single batch of solution from the ninth RFSA campaign, dissolved in January and February of this year, and two batches from the tenth campaign, dissolved in February, have been successfully processed. Following dissolution in Tank 6.4D, chloride was precipitated with mercurous ion added as the nitrate. The precipitate, Hg{sub 2}Cl{sub 2}, was concurrently removed with the gelatin floc via centrifugation. For each of these three batches processed, a set of duplicate samples was obtained from Tank 11.2 or from Tank 13.3, containing the head end product. The samples were preanalyzed by Laboratories Department for density and acidity to ensure them to be representative of the tank`s contents prior to chloride analysis by the Separations Technology Laboratory. Previous work indicated that in order to protect downstream canyon equipment from chloride attack, the chloride content of RFSA solutions should be less than 100 ppm. All batches from these two RFSA campaigns meet this criterion.
Date: March 8, 1988
Creator: Holcomb, H.P.
Partner: UNT Libraries Government Documents Department

234-5 Development Group - summary report, use of {open_quotes}AT{close_quotes} solution without evaporation

Description: A summary of work is presented from the 234-5 Development Group, September 1, 1950, with regard to the feasibility of transferring the plutonium processing solution, without evaporation, to the Purification Building. Critical factors identified were the concentration of the nitric acid and temperature.
Date: September 1, 1950
Creator: Lyon, W.L. & Facer, J.F.
Partner: UNT Libraries Government Documents Department

Composite electrodes for advanced electrochemical applications. Quarterly report for the period July 1 - September 30, 1999

Description: The electrochemical industry is one of the most highly energy-intensive industries today. However, there have been no significant advances in the electrodes that these industries use. The dimensionally stable anode (DSA), which ELTECH introduced under a license agreement, has been the industry standard for the past twenty-five years. But, DSAs are nearing the end of their technological prevalence. The principal problems with DSAs include high capital and operating cost, and the proprietary nature of the technology. In addition, DSAs experience problems that include contamination of the process solution by anode materials, failure when the electrocatalytic coating peels from under attack, generally low anode performance due to inherent limitations in operating current density, and short anode lifetime because of corrosion. The proposed innovation combines the low electrical resistance of copper with the corrosion resistance of electrically conductive diamond to achieve energy-efficient, long-lifetime electrodes for electrochemistry. The proposed work will ultimately develop a composite electrode that consists of a copper substrate, a conductive diamond coating, and a catalytic precious metal coating. The scope of the current work includes preparation, testing, and evaluation of diamond-coated titanium electrodes.
Date: October 1, 1999
Creator: Kovach, Chris
Partner: UNT Libraries Government Documents Department

Thermal Expansion and Hydration Behavior of PMMA Moulding Materials for LIGA Applications

Description: The thermal expansion coefficient, swelling characteristics and solute uptake kinetics of three PMMA molding materials (Perspex-CQ, Acrylite OP-1 and Solacryl 2750) are reported. Over the temperature range of 22 C to 50 C, all three materials exhibited similar CTE values of approximately 7.5 x 10{sup -5} C{sup -1}. Swelling characteristics, measured as the change in length of coupons were examined in three environments: deionized water, Ni Sulfamate plating solution and Ni Watts plating solution. Total swelling after {approx}150 hours of exposure was similar for all materials in each environment but were different for each environment examined: {approx}0.42% for de-ionized water, {approx} 0.30% for the Ni Sulfamate and {approx} 0.36% for the Ni-Watts plating solutions. Solute uptake kinetics were measured between 4 C and 50 C and the pre-exponential term (D{sub o}) and the activation energy (QD) are reported for each material in the three environments. Do values ranged between 0.07 and 0.45 cm{sup 2}/sec depending on the environment. Q{sub D} showed little variation, ranging between 4.1 and 4.4 x 10{sup 5} J/mole.
Date: February 1, 2003
Creator: Goods, Steven H.
Partner: UNT Libraries Government Documents Department

Caustic Precipitation of Plutonium and Uranium with Gadolinium as a Neutron Poison

Description: The caustic precipitation of plutonium (Pu) and uranium (U) from Pu and U-containing waste solutions has been investigated to determine whether gadolinium (Gd) could be used as a neutron poison for precipitation with greater than a fissile mass containing both Pu and enriched U. Precipitation experiments were performed using both process solution samples and simulant solutions with a range of 2.6-5.16 g/L U and 0-4.3:1 U:Pu. Analyses were performed on solutions at intermediate pH to determine the partitioning of elements for accident scenarios. When both Pu and U were present in the solution, precipitation began at pH 4.5 and by pH 7, 99% of Pu and U had precipitated. When complete neutralization was achieved at pH > 14 with 1.2 M excess OH{sup -}, greater than 99% of Pu, U, and Gd had precipitated. At pH > 14, the particles sizes were larger and the distribution was a single mode. The ratio of hydrogen:fissile atoms in the precipitate was determined after both settling and centrifuging and indicates that sufficient water was associated with the precipitates to provide the needed neutron moderation for Gd to prevent a criticality in solutions containing up to 4.3:1 U:Pu and up to 5.16 g/L U.
Date: October 18, 2005
Creator: VISSER, ANN E.; BRONIKOWSKI, MICHAEL G. & RUDISILL, TRACY S.
Partner: UNT Libraries Government Documents Department

Chloride content of dissolver solution from Rocky Flats alloy thirteenth campaign following head end treatment

Description: F-Canyon continues to obtain good chloride removal from Rocky Flats Alloy solution during head end treatment. One single batch of solution from the thirteenth alloy campaign, dissolved earlier this month, has been successfully processed. This was the first campaign to combine Rocky Flats Scrub Alloy (RFSA) with Rocky Flats Anode Heel Alloy (RFAHA) in the same dissolution solution (TA-2-1183). Following dissolution in Tank 6.4D, chloride was precipitated with mercurous ion added as the nitrate. The precipitate, Hg{sub 2}Cl{sub 2}, was concurrently removed with the gelatin floc via centrifugation. For this batch, a set of duplicate samples was initially obtained from Tank 11.2. However, due to repeated acid and density measurements by Laboratories, the volume of sample remaining was insufficient to permit chloride analysis. Samples of the same solution, now transferred to Tank 13.3, were analyzed. During the transfer, a 2% dilution occurred, but this error is not significant due to the larger error in the chloride analysis. For the single batch of RFSA-RFAHA material processed from the thirteenth campaign, the head end product contained 52 ppm ({micro}g/mL) chloride, a DF of 22. Relative standard deviation of the measurement was {+-}6 ppm (n = 4) for a precision of {+-}12%.
Date: September 20, 1988
Creator: Holcomb, H. P.
Partner: UNT Libraries Government Documents Department

Chloride content of Rocky Flats scrub alloy eleventh campaign solution following head end treatment

Description: A single batch of dissolver solution from the eleventh Rocky Flats Scrub Alloy (RFSA) campaign has been analyzed for chloride content following head end treatment to reduce its concentration. Scrub alloy buttons were dissolved in Tank 6.4D during May. In subsequent head end processing, chloride was precipitated with mercurous ion added as the nitrate. The precipitate, Hg{sub 2}Cl{sub 2}, was concurrently removed with the gelatin floc via centrifugation. Duplicate samples from Tank 11.2, containing the head end product, produced excellent agreement between their density measurements, acid analyses, and gross alpha activities, indicating them to be truly representative of the tank`s contents. Duplicate aliquots from each of these solutions were analyzed using the turbidimetric chloride method developed in the Separations Technology Laboratory. These resulted in an average chloride value of 41 ppm ({micro}g/mL) chloride for the head end product. Relative standard deviation of the measurement was {+-}4 ppm (n = 4), a precision of {+-}10%. Such a variance is normal at this low chloride level. Since initial chloride values prior to head end averaged 1455 ppm (0.041M), as analyzed by Laboratories Department, a chloride DF of approximately 35 was obtained. Such a reduced chloride level (to less than 100 ppm) in the treated solution will permit further canyon processing with minimal corrosion.
Date: June 30, 1988
Creator: Holcomb, H. P.
Partner: UNT Libraries Government Documents Department

Solids formation on filtrate neutralization

Description: The Separations Technology Laboratory was requested to study what happens when a filtrate solution, which will be a F B-Line product, is neutralized with sodium hydroxide. The primary concern was the formation of solids that could cause damage in pump seals, resulting in their failure. The results of these experiments indicate that under process conditions, granular, crystalline sodium fluoride will be produced by rapid neutralization of the filtrate solution with 50% NaOH plus a 25 volume percent excess. Postprecipitation of sodium oxalate-sodium fluoride and its accumulation can occur over a three-week storage period of the neutralized filtrate. Such solids could pose operational problems from pump seal abrasion and potential failure caused by them.
Date: May 26, 1988
Creator: Holcomb, H.P.
Partner: UNT Libraries Government Documents Department

Chloride content of Rocky Flats scrub alloy twelfth campaign solution following head end treatment

Description: A single batch of dissolver solution from the twelfth Rocky Flats Scrub Alloy (RFSA) campaign has been analyzed for chloride content following head end treatment to reduce its concentration. Scrub alloy buttons were dissolved in Tank 6.4D during July. In subsequent head end processing, chloride was precipitated with mercurous ion added as the nitrate. The precipitate, Hg{sub 2}Cl{sub 2}, was co-removed with the gelatin floc via centrifugation. Duplicate samples from Tank 11.2, containing the head end product, produced excellent agreement between their density measurements and acid analyses, indicating them to be truly representative of the tank`s contents. Duplicate aliquots from each of these solutions were analyzed using the turbidimetric chloride method developed in the Separations Technology Laboratory. These resulted in an average chloride value of 53 ppm ({micro}g/mL) chloride for the head end product. Relative standard deviation of the measurement was {+-}6 ppm (n = 4), a precision of {+-}11%. Such a variance is normal at this low chloride level. Since initial chloride values prior to head end averaged 1365 ppm (0.0385M), as analyzed by Laboratories Department, a chloride DF of approximately 26 was obtained. Such a reduced chloride level (to less than 100 ppm) in the treated solution will permit further canyon processing with minimal corrosion.
Date: August 8, 1988
Creator: Holcomb, H. P.
Partner: UNT Libraries Government Documents Department

PFP solution stabilization

Description: This Functional Design Criteria (FDC) addresses remediation of the plutonium-bearing solutions currently in inventory at the Plutonium Finishing Plant (PFP). The recommendation from the Environmental Impact Statement (EIS) is that the solutions be treated thermally and stabilized as a solid for long term storage. For solutions which are not discardable, the baseline plan is to utilize a denitration process to stabilize the solutions prior to packaging for storage.
Date: April 30, 1996
Creator: Aftanas, B.L.
Partner: UNT Libraries Government Documents Department

Simultaneous measurements of plutonium and uranium in spent-fuel dissolver solutions

Description: The authors have studied the isotope dilution gamma-ray spectrometry (IDGS) technique for simultaneous measurements of elemental concentrations and isotopic compositions for both plutonium and uranium in input spent-fuel dissolver solutions at a reprocessing plant. The technique under development includes both sample preparation and analysis methods. For simultaneous measurements of both plutonium and uranium, a critical issue is to develop a new method to keep both plutonium and uranium in the sample after they are separated from fission products. Furthermore, it is equally important to improve the analysis method so that the precision and accuracy of the plutonium analysis remain unaffected while uranium is retained in the sample. To keep both plutonium and uranium in the sample for simultaneous measurements, extraction chromatography is being studied and shows promise to achieve the goal of cosegregation of the plutonium and uranium. The technique uses U/TEVA{center_dot}Spec resin to separate fission products and recover both uranium and plutonium in the resin from dissolver solutions for subsequent measuring using high-resolution gamma-ray spectrometry. Owing to the fact that the U/Pu ratio is altered during the fission product separation phase, it is necessary to develop a method which could accurately correct for this effect. Such a method was developed using the unique decay properties of {sup 241}Pu to {sup 237}U and shows considerable promise in allowing for accurate determination of the {sup 235}U concentrations before the chemical extraction.
Date: November 1, 1997
Creator: Li, T.K.; Kuno, T.; Kitagawa, O.; Sato, S.; Kurosawa, A. & Kuno, Y.
Partner: UNT Libraries Government Documents Department

Fate of soluble uranium in the I{sub 2}/KI leaching process for mercury removal

Description: General Electric Corporation has developed an extraction and recovery system for mercury, based upon the use of iodine (oxidant) and iodide ion (complexing agent). This system has been proposed for application to select mercury-contaminated mixed waste (i.e., waste containing radionuclides as well as other hazardous constituents), which have been generated by historic activities in support of US Department of Energy (DOE) missions. This system is compared to a system utilizing hypochlorite and chloride ions for removal of mercury and uranium from a sample of authentic mixed waste sludge. Relative to the hypochlorite (bleach) system, the iodine system mobilized more mercury and less uranium from the sludge. An engineering flowsheet has been developed to treat spent iodine-containing extraction medium, allowing the system to be recycled. The fate of soluble uranium in this series of treatment unit operations was monitored by tracing isotopically-enriched uranyl ion into simulated spent extraction medium. Treatment with use of elemental iron is shown to remove > 85% of the traced uranium while concurrently reducing excess iodine to the iodide ion. The next unit operation, adjustment of the solution pH to a value near 12 by the addition of lime slurry to form a metal-laden sludge phase (an operation referred to as lime-softening), removed an additional 57% of soluble uranium activity, for an over-all removal efficiency of {approximately} 96%. However, the precipitated solids did not settle well, and some iodide reagent is held up in the wet filtercake.
Date: September 1, 1997
Creator: Bostick, W.D.; Davis, W.H. & Jarabek, R.J.
Partner: UNT Libraries Government Documents Department

Equilibrium characteristics of tartrate and EDTA-based electroless copper deposition baths

Description: Electroless deposition of copper is being used for a variety of applications, one of them being the development of seed metallic layers on non-metals, which are widely used in electronic circuitry. Solution equilibrium characteristics of two electroless copper baths containing EDTA and tartrate as the complexing agents were studied as functions of pH, chelating agent and metal ion concentrations. Equilibrium diagrams were constructed for both cu-tartrate and Cu-EDTA systems. It was determined that copper is chiefly complexed as Cu(OH){sub 2}L{sub 2}{sup {minus}4} in the tartrate bath, and as CuA{sup {minus}2} in the EDTA bath, where L and A are the complexing tartrate and EDTA ligands, respectively. The operating ranges for electroless copper deposition were identified for both baths. Dependence of Cu(OH){sub 2} precipitation on the pH and species concentrations was also studied for these systems.
Date: August 1, 1997
Creator: Ramasubramanian, M.; Popov, B.N.; White, R.E. & Chen, K.S.
Partner: UNT Libraries Government Documents Department

Test procedure for anion exchange testing with Argonne 10-L solutions

Description: Four anion exchange resins will be tested to confirm that they will sorb and release plutonium from/to the appropriate solutions in the presence of other cations. Certain cations need to be removed from the test solutions to minimize adverse behavior in other processing equipment. The ion exchange resins will be tested using old laboratory solutions from Argonne National Laboratory; results will be compared to results from other similar processes for application to all plutonium solutions stored in the Plutonium Finishing Plant.
Date: May 17, 1995
Creator: Compton, J.A.
Partner: UNT Libraries Government Documents Department

Analysis of Americium in Transplutonium Process Solutions

Description: One of the more difficult analyses in the transplutonium field is the determination of americium at trace levels in a complex matrix such as a process dissolver solution. Because of these conditions a highly selective separation must precede the measurement of americium. The separation technique should be mechanically simple to permit remote operation with master-slave manipulators. For subsequent americium measurement by the mass spectroscopic isotopic-dilution technique, plutonium and curium interferences must also have been removed.
Date: March 9, 2001
Creator: Ferguson, R.B.
Partner: UNT Libraries Government Documents Department

Solution monitoring: Quantitative benefits to safeguards

Description: This paper investigates how SM (essentially continuous monitoring of solution level, density, and temperature in all key process tanks) can improve loss detection in a formal statistical sense. The authors use a simulation code developed at Los Alamos (FACSIM) to simulate data from the Rokkasho Reprocessing Plant (RRP), which is now under construction in Japan. They show the possibility of reducing the effect of systematic errors by using solution monitoring data to calculate bias corrections. They divide the effort into 4 activities for a 3-tank system and for a more realistic 15-tank system. The authors say a tank is in wait mode if its level change is due only to measurement error. Otherwise, a tank is in transfer mode. The 4 activities are (1) monitor each tank for volume loss during each wait mode, (2) monitor each tank for mass loss during each wait mode, (3) monitor each tank for volume loss during each transfer mode, and (4) monitor each tank for mass loss during each transfer mode. The success of this effort will depend largely on the performance of the authors` proposed bias corrections to the volume measurements. To apply bias corrections, the authors require that some reasonable number of transfers (for example, 20) are known to have no true loss. The effectiveness of the technique will depend on the relative sizes of the random and systematic errors involved because the main outcome is a reduction of the systematic error variances. If there are large variations in true (legitimate) temporary losses such as pipe holdup that would add to the random error variance in this model, the effectiveness will be reduced. Even in such cases the authors show there can be improved protracted loss detection and will definitely be improved abrupt loss detection.
Date: October 1, 1997
Creator: Burr, T.L.; Coulter, C.A. & Wangen, L.E.
Partner: UNT Libraries Government Documents Department

A method and apparatus for sizing and separating warp yarns

Description: A slashing process for preparing warp yarns for weaving operations includes the steps of sizing and/or desizing the yarns in an acoustic resonance box and separating the yarns with a leasing apparatus comprised of a set of acoustically agitated lease rods. The sizing step includes immersing the yarns in a size solution contained in an acoustic resonance box. Acoustic transducers are positioned against the exterior of the box for generating an acoustic pressure field within the size solution. Ultrasonic waves that result from the acoustic pressure field continuously agitate the size solution to effect greater mixing and more uniform application and penetration of the size onto the yarns. The sized yarns are then separated by passing the warp yarns over and under lease rods. Electroacoustic transducers generate acoustic waves along the longitudinal axis of the lease rods, creating a shearing motion on the surface of the rods for splitting the yarns.
Date: December 1, 1997
Creator: Sheen, Shuh-Haw; Chien, Hual-Te; Raptis, Apostolos C. & Kupperman, David S.
Partner: UNT Libraries Government Documents Department

Criticality Safety Evaluation Report for the Cold Vacuum Drying (CVD) Facilities Process Water Handling System

Description: This report addresses the criticality concerns associated with process water handling in the Cold Vacuum Drying Facility. The controls and limitations on equipment design and operations to control potential criticality occurrences are identified.
Date: August 10, 2000
Creator: KESSLER, S.F.
Partner: UNT Libraries Government Documents Department

Small-Column Cesium Ion Exchange Elution Testing of Spherical Resorcinol-Formaldehyde

Description: This report summarizes the work performed to evaluate multiple, cesium loading, and elution cycles for small columns containing SRF resin using a simple, high-level waste (HLW) simulant. Cesium ion exchange loading and elution curves were generated for a nominal 5 M Na, 2.4E-05 M Cs, 0.115 M Al loading solution traced with 134Cs followed by elution with variable HNO3 (0.02, 0.07, 0.15, 0.23, and 0.28 M) containing variable CsNO3 (5.0E-09, 5.0E-08, and 5.0E-07 M) and traced with 137Cs. The ion exchange system consisted of a pump, tubing, process solutions, and a single, small ({approx}15.7 mL) bed of SRF resin with a water-jacketed column for temperature-control. The columns were loaded with approximately 250 bed volumes (BVs) of feed solution at 45 C and at 1.5 to 12 BV per hour (0.15 to 1.2 cm/min). The columns were then eluted with 29+ BVs of HNO3 processed at 25 C and at 1.4 BV/h. The two independent tracers allowed analysis of the on-column cesium interaction between the loading and elution solutions. The objective of these tests was to improve the correlation between the spent resin cesium content and cesium leached out of the resin in subsequent loading cycles (cesium leakage) to help establish acid strength and purity requirements.
Date: October 21, 2011
Creator: Brown, Garrett N.; Russell, Renee L. & Peterson, Reid A.
Partner: UNT Libraries Government Documents Department