Preparation of acid standards for and determination of free acid in concentrated plutonium-uranium solutions

Ryan, J.L.; Bryan, G.H.; Burt, M.C.; Costanzo, D.A.

doi:10.1021/ac00284a055

Cited by 16 publications

(12 citation statements)

References 18 publications

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“…Since those measurements, a study was made and a free acid analysis method 3.3 . developed and reported (Ryan 1985). This has significantly reduced uncertainties in the analysis for free acid.…”

Section: Sources Of Errormentioning

confidence: 93%

Criticality Experiments with Mixed Plutonium and Uranium Nitrate Solution at a Plutonium Fraction of 0.5 in Annular Cylindrical Geometry

Lloyd¹

1988

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S526 SUMMARYA series of critical experiments was completed with mixed plutonium-uranium solutions having Pu/(Pu + U) ratios of approximately 0.5. These experiments were a part of the Criticality Data Development Program between the United States Department of Energy (USDOE), and the Power Reactor and Nuclear Fuel Development Corporation (PNC) of Japan. A complete description of, and data from, the experiments are included in this report. The experiments were performed with mixed plutonium-uranium solutions in annular cylindrical geometry. The measurements were made with a water reflector. The central region included a concrete annular cylinder containing s 4 c. Interior to the concrete insert was a stainless steel bottle containing plutonium-uranium solution. The concentration of the solution in the annular region was varied from 116 to 433 g (Pu + U)/liter. The ratio of plutonium to total heavy metal (plutonium plus uranium) was 52% for all experiments.iii CONTENTS

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Section: Sources Of Errormentioning

confidence: 93%

Criticality Experiments with Mixed Plutonium and Uranium Nitrate Solution at a Plutonium Fraction of 0.5 in Annular Cylindrical Geometry

Lloyd¹

1988

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“… HNO 3 concentration by Raman spectroscopy; supplemented with titration in ammonium oxalate complexing buffer. [23]…”

Section: Slurry Withdrawal Linementioning

confidence: 99%

Design of the Laboratory-Scale Plutonium Oxide Processing Unit in the Radiochemical Processing Laboratory

Lumetta

Meier

Tingey

et al. 2015

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This report describes a design for a laboratory-scale capability to produce plutonium oxide (PuO 2) for use in identifying and validating nuclear forensics signatures associated with plutonium production, as well as for use as exercise and reference materials. This capability will be located in the Radiochemical Processing Laboratory at the Pacific Northwest National Laboratory. The key unit operations are described, including PuO 2 dissolution, purification of the Pu by ion exchange, precipitation, and reconversion to PuO 2 by calcination. v Summary The National Technical Nuclear Forensics Center (NTNFC) within the Domestic Nuclear Detection Office (DNDO) of the Department of Homeland Security (DHS) has funded Pacific Northwest National Laboratory (PNNL) to establish a laboratory-scale (up to 200 g Pu per batch) capability to produce plutonium oxide (PuO 2) for use in identifying and validating nuclear forensics signatures associated with plutonium production, as well as for use as exercise and reference materials. This capability is being installed in Room 604 in the Radiochemical Processing Laboratory (RPL). The key unit operations for producing PuO 2 are as follows. The feed plutonium material is received in the RPL in oxide form. The as-received oxide is dissolved in nitric acid media (with fluoride added as needed). The resulting solution is subjected to ion exchange to remove impurities from the plutonium stream, and then the plutonium is precipitated in the form of a salt (e.g., oxalate, peroxide, or hydroxide). Finally, this Pu salt is converted back to PuO 2 by heating (calcining). In order to make this capability a useful tool for identifying and validating nuclear forensics signatures, the system is designed to be flexible, allowing variations in the different process parameters (e.g., temperature, manner of reagent addition, or type of precipitating agent). This report describes the laboratory-scale PuO 2 production capability being established at PNNL. The key features include:  Plutonium oxide is received at the RPL and 200 g aliquots are transferred to a glovebox in RPL Room 604 for processing.  The PuO 2 is dissolved in nitric acid media. If necessary, fluoride (in the form of calcium fluoride or hydrofluoric acid) is added to aid in dissolving the PuO 2.  The plutonium solution is clarified by filtration and then purified by anion exchange using Reillex HPQ ® anion-exchange resin, or another suitable anion-exchange resin.  Although the design allows for a variety of plutonium precipitation steps, the design is based primarily on Pu(III) oxalate [Pu 2 (C 2 O 4) 3 •10H 2 O] precipitation. The purified Pu solution is adjusted to the +3 oxidation state with ascorbic acid, then is treated with oxalic acid to precipitate Pu 2 (C 2 O 4) 3 •10H 2 O.  The Pu 2 (C 2 O 4) 3 •10H 2 O is calcined in a muffle furnace to convert it to PuO 2.  The PuO 2 product is packaged and distributed as directed by the NTNFC. Functional descriptions are provided for each unit operation, and the various requirements f...

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“…From Primm's analysis it was found that the principal uncertainty, or error, was caused by the uncertainty in the free acid values. Since then, a study was made of chemical analysis methods and a free acid analysis method developed and reported (Ryan 1985). This has $ignificantly reduced uncertainties in the analysis for free acid.…”

Section: Sources Of Errormentioning

confidence: 99%

Criticality Experiments with Mixed Plutonium and Uranium Nitrate Solution at a Plutonium Fraction of 0.4 in Slab and Cylindrical Geometry

Lloyd¹

1988

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SUMMARYA series of critical experiments was completed with mixed plutonium-uranium solutions having Pu/(Pu + U) ratios of approximately 0.4. These experiments were a part of the Criticality Data Development Program between the United States Department of Energy (USDOE), and the Power Reactor and Nuclear Fuel Development Corporation (PNC) of Japan. A complete description of, and data from, the experiments are included in this report. The experiments were performed with mixed plutonium-uranium solutions in cylinqrical and slab geometries and included measurements with a water reflector, a concrete reflector, and without an added reflector. The concentration was varied from 105 to 436 g (Pu + U)/liter. The ratio of plutonium to total heavy metal (plutonium plus uranium) was 0.4 for all experiments.iii CONTENTS

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Preparation of acid standards for and determination of free acid in concentrated plutonium-uranium solutions

Cited by 16 publications

References 18 publications

Criticality Experiments with Mixed Plutonium and Uranium Nitrate Solution at a Plutonium Fraction of 0.5 in Annular Cylindrical Geometry

Criticality Experiments with Mixed Plutonium and Uranium Nitrate Solution at a Plutonium Fraction of 0.5 in Annular Cylindrical Geometry

Design of the Laboratory-Scale Plutonium Oxide Processing Unit in the Radiochemical Processing Laboratory

Criticality Experiments with Mixed Plutonium and Uranium Nitrate Solution at a Plutonium Fraction of 0.4 in Slab and Cylindrical Geometry

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