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Plutonium Nitrate Shipping Investigation

Description: With the AEC complex there has been a long history of shipper-receiver assay differences in the transfer of plutonium nitrate solutions. Since the AEC is considering establishing plutonium nitrate as one of the chemical forms of plutonium for Commission purchase of privately produced plutonium, it is necessary that the shipper-receiver problem be resolved. The program formulated by Rocky Flats for doing this, and the results obtained to date, are discussed. (auth)
Date: September 1, 1963
Creator: Miner, F. J. & Byrne, J. T.
Partner: UNT Libraries Government Documents Department

Criticality experiments with planar arrays of three-liter bottles containing plutonium nitrate solution

Description: The objective of these experiments was to provide benchmark data to validate calculational codes used in critically safety assessments of plant configurations. Arrays containing up to as many as sixteen three-liter bottles filled with plutonium nitrate were used in the experiments. A split-table device was used in the final assembly of the arrays. Ths planar arrays were reflected with close fitting plexiglas on each side and on the bottom but not the top surface. The experiments addressed a number of factors effecting criticality: the critical air gap between bottles in an array of fixed number of bottles, the number of bottles required for criticality if the bottles were touching, and the effect on critical array spacing and critical bottle number due to the insertion of an hydrogeneous substance into the air gap between bottles. Each bottle contained about 2.4l of Pu(NO{sub 3}){sub 4} solution at a Pu concentration of 105g Pu/l, with the {sup 240}Pu content being 2.9 wt% at a free acid molarity H{sup +} of 5.1. After the initial series of experiments were performed with bottles separated by air gaps, plexiglas shells of varying thicknesses were placed around each bottle to investigate how moderation between bottles affects both the number of bottles required for criticality and the critical spacing between each bottle. The minimum of bottles required for criticality was found to be 10.9 bottles, occurring for a square array with bottles in contact. As the bottles were spaced apart, the critical number increased. For sixteen bottles in a square array, the critical separation between surfaces in both x and y direction was 0.96 cm. The addition of plexiglas around each bottle decreased the critical bottle number, compared to those separated in air, but the critical bottle number, even with interstitial plastic in place was always greater than ...
Date: January 1, 1985
Creator: Durst, B.M.; Clayton, E.D. & Smith, J.H.
Partner: UNT Libraries Government Documents Department

Parameters in the Conversion of Plutonium Nitrate to Plutonium Trichloride by a Direct Calcination--Fluid Bed Chlorination Process

Description: Results of studies of the known parameters for direct calcination of plutonium nitrate in an agitated bed and conversion of PuO/sub 2/ to PuCl/sub 3/ by fluid bed processes are presented. A description of the processes and the demonstration equipment is included. The study of variables is discussed along with the parameters and plans for demonstration runs. (J.R.D.)
Date: May 31, 1961
Creator: Rasmussen, M. J.; Stiffler, G. L. & Hopkins, H. H., Jr.
Partner: UNT Libraries Government Documents Department


Description: A colorimeter is described that can be used to monitor process solutions continuously for uranyl nitrate or plutonium nitrate concentration. The instrument was tested under plant conditions in the concentration range from 0.1 to 70 grams of uranium per liter and 0.1 to 10 grams of plutonium per liter. The instrument error was plus or minus 1% of the span, but errors of 15 to 20% can be caused by other variables such as acidity and other salts present. (auth)
Date: March 1, 1960
Creator: Colvin, D.W.
Partner: UNT Libraries Government Documents Department

New spectroscopic studies of plutonium (IV) nitrate complex formation in solution

Description: Spectrophotometric titrations of Pu(IV) with HNO{sub 3} were conducted in a series of aqueous HClO{sub 4} solutions ranging ionic strength from 2 to 19 mol/kg on the molality scale. The Pu f-f absorption spectra in the visible and near IR range were deconvoluted into spectra of Pu{sup 4+}(aq), Pu(NO{sub 3}){sup 3+} and Pu(NO{sub 3}){sub 2}{sup 2+} complexes and their formation constants as functions of ionic strength. When corrected for the incomplete dissociation of nitric acid, these formation constants exhibit smooth increases with ionic strength from 5 to 19 mol/kg.
Date: June 1, 1997
Creator: Berg, J.M.; Veirs, D.K. & Vaughn, R.B.
Partner: UNT Libraries Government Documents Department

Procedure for plutonium determination using Pu(VI) spectra

Description: This document describes a simple spectrophotometric method for determining total plutonium in nitric acid solutions based on the spectrum of Pu(VI). Plutonium samples in nitric acid are oxidized to Pu(VI) with Ce(IV) and the net absorbance at the 830 nm peak is measured.
Date: September 1, 1996
Creator: Walker, L.F.; Temer, D.J. & Jackson, D.D.
Partner: UNT Libraries Government Documents Department

Subcritical measurements with a cylindrical tank of Pu-U nitrate

Description: This series of measurements with a mixed Pu-U nitrate solution (280 g Pu/liter, 180 g U/liter) in a 35.54-cm-diam cylindrical tank provides a wide variety of experimental data for subcritical configurations that can be used to verify calculational methods and nuclear data. The Pu contained 7.85 wt% {sup 240}Pu and the uranium was natural uranium. The measurements performed were: inverse count rate, prompt neutron decay constants, inverse kinetics, and frequency analysis by the {sup 252}Cf source driven method. These data are presented in sufficient detail that the results of the experiments can be calculated directly. For purposes of extrapolating to the delayed critical height the ratio of spectral densities was linear with height and thus provided the best estimate of critical height.
Date: April 1, 1997
Creator: Mihalczo, J.T.; Valentine, T.E. & King, W.T.
Partner: UNT Libraries Government Documents Department

Plutonium(IV) oxalate precipitation and calcination process for plutonium nitrate to oxide conversion

Description: The Plutonium(IV) Oxalate Precipitation and Calcination Process for converting plutonium nitrate to plutonium oxide is described for a 100-kg plutonium per day (Pu/day/ throughput facility. Block flow diagrams, equipment flowsheets, and stream material balances are included. Advantages and disadvantages of the process, additional research and development necessary, and history of the process are also discussed. This report is one of a series describing various processes for converting plutonium nitrate to oxide. This information in this report should be used when comparing the various processes, and as a starting point for development of a prototype or plant-scale facility.
Date: July 26, 1978
Creator: Greintz, R.M. & Neal, D.H.
Partner: UNT Libraries Government Documents Department

Criticality experiments with mixed plutonium and uranium nitrate solution at a plutonium fraction of 0.4 in slab geometry

Description: R. C. Lloyd of PNL has completed and published a series of critical experiments with mixed plutonium- uranium nitrate solutions (Reference 1). This series of critical experiments was part of an extensive program jointly sponsored by the U. S. Department of Energy (DOE) and the Power Reactor and Nuclear Fuel Development Corporation (PNC) of Japan and was carried out in the mid-1980`s. The experiments evaluated here (published as Report PNL-6327) were performed with mixed plutonium- uranium nitrate solution in a variable thickness slab tank with two 106.7 cm square sides and a width that could be varied from 7.6 to 22.8 cm. The objective of these experiments was to obtain experimental data to permit the validation of computer codes for criticality calculations and of cross-section data to minimize the uncertainties inherent therein, so that facility safety, efficiency, and reliability could be enhanced. The concentrations of the solution were about 105, 293, and 435 g(Pu+U)/liter with a ratio of plutonium to total heavy metal (plutonium plus uranium) of about 0. 40 for all eight experiments. Four measurements were made with a water reflector, and four with no reflector. Following the publication of the initial PNL reports, considerable effort was devoted to an extensive reevaluation of this series of experiments by a collaboration of researchers from ORNL, PNL, and PNC (Reference 2). Their work resulted in a more accurate description of the ``as built`` hardware configuration and the materials specifications. For the evaluations in this report, the data published in Reference 2 by Smolen et al. is selected to supersede the original PNL report. Eight experiments have been evaluated and seven (063, 064, 071, 072, 074, 075, and 076) provide benchmark criticality data. Experiment 073 could not achieve criticality within vessel height limitations.
Date: September 1, 1997
Creator: Pohl, B.A. & Keeton, S.C.
Partner: UNT Libraries Government Documents Department

Integrating safety and health during deactiviation: With lessons learned from PUREX

Description: This report summarizes an integrated safety and health approach used during facility deactivation activities at the Department of Energy (DOE) Plutonium-Uranium Extraction (PUREX) Facility in Hanford, Washington. Resulting safety and health improvements and the potential, complex-wide application of this approach are discussed in this report through a description of its components and the impacts, or lessons-learned, of its use during the PUREX deactivation project. As a means of developing and implementing the integrated safety and health approach, the PUREX technical partnership was established in 1993 among the Office of Environment, Safety and Health`s Office of Worker Health and Safety (EH-5); the Office of Environmental Management`s Offices of Nuclear Material and Facility Stabilization (EM-60) and Compliance and Program Coordination (EM-20); the DOE Richland Operations Office; and the Westinghouse Hanford Company. It is believed that this report will provide guidance for instituting an integrated safety and health approach not only for deactivation activities, but for decommissioning and other clean-up activities as well. This confidence is based largely upon the rationality of the approach, often termed as common sense, and the measurable safety and health and project performance results that application of the approach produced during actual deactivation work at the PUREX Facility.
Date: September 29, 1995
Partner: UNT Libraries Government Documents Department

Sorption of Pu(IV) from nitric acid by bifunctional anion-exchange resins

Description: Anion exchange is attractive for separating plutonium because the Pu(IV) nitrate complex is very strongly sorbed and few other metal ions form competing anionic nitrate complexes. The major disadvantage of this process has been the unusually slow rate at which the Pu(IV) nitrate complex is sorbed by the resin. The paper summarizes the concept of bifunctional anion-exchange resins, proposed mechanism for Pu(IV) sorption, synthesis of the alkylating agent, calculation of K{sub d} values from Pu(IV) sorption results, and conclusions from the study of Pu(IV) sorption from 7M nitric acid by macroporous anion-exchange resins including level of crosslinking, level of alkylation, length of spacer, and bifunctional vs. monofunctional anion-exchange resins.
Date: June 1, 1999
Creator: Bartsch, R.A.; Zhang, Z.Y.; Elshani, S.; Zhao, W.; Jarvinen, G.D.; Barr, M.E. et al.
Partner: UNT Libraries Government Documents Department

Notes Pertaining to Recuplex Product Evaporation

Description: A red-brown liquid formed during the evaporation of simulated Recuplex product solutions containing plutonium, nitric acid, carbon tetrachloride, and tributyl phosphate (TBP). The liquid is soluble in carbon tetrachloride. Concentration of solutions containing a TBP to plutonyl nitrate weight ratio of 0.15 or greater to a pot temperature of 150 deg C caused reactions which produced enough heat to bring the pot contents to a red heat with copious evolution of gases. Evaporation path curves and boiling point data were obtained from batch evaporations with minimum reflux and are presented. Polymeric plutonium(IV) was formed upon concentrating plutonium nitrate solutions of low nitric acid content. The region of polymer formation was defined and is presented. (auth)
Date: April 28, 1954
Creator: Pugh, R. A.
Partner: UNT Libraries Government Documents Department

Amine Extraction of Plutonium From Nitric Acid Solutions Loading and Stripping Experiments

Description: Information is presented on a suitable amine processing system for plutonium nitrate. Experiments with concentrated plutonium nitrate solutions show that trilaurylamine (TLA) - xylene solvent systems did not form a second organic phase. Experiments are also reported with tri-noctylamine (TnOA)-xylene and TLA-Amsco - octyl alcohol. Two organic phases appear in both these systems at high plutonium nitrate concentrations. Data are tabulated from loading and stripping experiments. (J.R.D.)
Date: January 19, 1961
Creator: Wilson, A. S.
Partner: UNT Libraries Government Documents Department

Production test 231-12: Recovery of americium. Final report

Description: In response to the need for isolating small quantities of americium for employment in research studies, principally at laboratories not connected with the Hanford Atomic Products Operation, a program was formulated to accomplish this at minimum cost and disturbance to plutonium production. This report describes the operations employed and the results obtained in the isolation of americium from aged plutonium nitrate solution utilizing the Isolation Building process equipment.
Date: March 2, 1954
Creator: Packer, G.V.
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

Dried plutonium nitrate decontamination using HNO{sub 3} or Freon 113

Description: A request was made of the Separations Technology Laboratory to perform tests to determine the relative effectiveness of Freon 113 and 18% (3.15M) nitric acid on removing dried plutonium nitrate from Hypalon{reg_sign} gloves destined for use in F B-Line. Freon 113 was very inefficient for removing dried plutonium nitrate under conditions of moderate agitation of the liquid in contact with the dried compound. Nitric acid proved to be an excellent agent for decontaminating purposes for both the gloves and for the Pyrex glass. In tests conducted on the glass or on the gloves on which dried plutonium nitrate had not been removed by Freon 113, followup with nitric acid efficiently removed the residual plutonium nitrate. Tests were also conducted to give some measure of the resistance of the Hypalon glove to continuous contact with 18% HNO{sub 3} or with Freon 113. Following two weeks` immersion, there was little physical difference noted from the starting material, except the glove piece immersed in the Freon underwent an 8% weight gain.
Date: February 4, 1988
Creator: Holcomb, H. P.
Partner: UNT Libraries Government Documents Department

Critical mass studies of plutonium solutions

Description: The chain reacting conditions for plutonium nitrate in water solution have been examined experimentally for a variety of sizes of spheres and cylinders. The effects on the critical mass of the displacement of hydrogen and the addition of poisons to the fuel were measured in water tamped and bare reactors. In this report the data obtained in the investigation is presented graphically and in tables. Some preliminary analysis has been made yielding the results: (i) the absorption cross-section of Pu{sup 240} is 925 {plus_minus} 200 barns and (ii) the minimum critical mass of Pu{sup 239} in water is 510 grams at concentration of about 33 grams per liter.
Date: May 19, 1952
Creator: Kruesi, F.E.; Erkman, J.O. & Lanning, D.D.
Partner: UNT Libraries Government Documents Department

Production Test 231-10 Supplement B process evaluation-production of concentrated plutonium nitrate solution in Building 231: Transfer to and processing in Building 234-5. Final report

Description: All of the 231 Building final product was prepared for off-site shipment prior to the startup of the 234-5 Building. The evaporator (S-1) effluent, a solution approximately 10 molar in nitric acid with plutonium concentration of 275 grams/liter, was dried within the shipping container (sample can) to a solid cake. The purpose of this drying operation was to minimize personnel contamination and/or loss of product during shipment. The dried cake was redissolved in water before further purification steps could be performed. The procedures for testing the purification of AT solution as recommended by the development group (6) were presented in Production Test 231-10 Supplement B. Production Test 231-10 Supplement B was initiated to establish the procedures for the precipitation of Plutonium (III) Oxalate in Plant equipment from AT solutions. The current report is written to provide a history of: Work done and data collected during the test, and Conclusions and Recommendations obtained from studies of the data.
Date: October 3, 1951
Creator: Kerr, W.B.
Partner: UNT Libraries Government Documents Department

CSER 00-003 Criticality Safety Evaluation report for PFP Magnesium Hydroxide Precipitation Process for Plutonium Stabilization Glovebox 3

Description: This Criticality Safety Evaluation Report analyzes the stabilization of plutonium/uranium solutions in Glovebox 3 using the magnesium hydroxide precipitation process at PFP. The process covered are the receipt of diluted plutonium solutions into three precipitation tanks, the precipitation of plutonium from the solution, the filtering of the plutonium precipitate from the solution, the scraping of the precipitate from the filter into boats, and the initial drying of the precipitated slurry on a hot plate. A batch (up to 2.5 kg) is brought into the glovebox as plutonium nitrate, processed, and is then removed in boats for further processing. This CSER establishes limits for the magnesium hydroxide precipitation process in Glovebox 3 to maintain criticality safety while handling fissionable material.
Date: July 13, 2000
Creator: LAN, J.S.
Partner: UNT Libraries Government Documents Department