Small-Scale Testing of Plutonium (Iv) Oxalate Precipitation and Calcination to Plutonium Oxide to Support the Mox Feed Mission

Crowder, Mark L.; Pierce, Robert A.; Scogin, J. H.; Daniel, G.; King, William D.

doi:10.2172/1044791

Cited by 10 publications

(9 citation statements)

References 2 publications

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“…Demonstrations of the precipitation process planned for HB-Line was demonstrated and documented in SRNL-STI-2012-00338 and SRNL-STI-2012-00422. [4][5] In this study, filtration testing was performed using plutonium oxalate prepared in nominally 3 g batches using Pu purified by anion exchange. Conditions for the precipitation targeted the oxalate addition time and digestion time expected in HB-Line.…”

Section: Methodsmentioning

confidence: 99%

“…The precipitation process used in these experiments followed the process demonstrated by SRNL which is documented in SRNL-STI-2012-00338 and SRNL-STI-2012-00422. [4][5] All precipitations occurred at 50 °C ± 3 °C with continuous stirring at 350 RPM. A 100-mL volume of the purified Pu stock solution was used in each precipitation.…”

Section: Precipitation and Filtration Of Plutonium Oxalatementioning

confidence: 99%

“…On closer inspection, Figure 3-12 shows at a 3000x magnification that each cube is layered, as observed in previous work. [4][5] The average particle size for the solids collected on the 0.1 μm filter for both the 1-and 4-day aged initial filtrate solution has been determined by applying the program Pixcavator 1A, version 6.0. The results from the Pixcavator program are shown in Table 3-5.…”

Section: Particle Size Analysismentioning

confidence: 99%

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Determination of filter pore size for use in HB line phase II production of plutonium oxide

Shehee

Crowder

Rudisill

2014

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H-Canyon and HB-Line are tasked with the production of plutonium oxide (PuO 2) from a feed of plutonium (Pu) metal. The PuO 2 will provide feed material for the Mixed Oxide (MOX) Fuel Fabrication Facility. After dissolution of the Pu metal in H-Canyon, plans are to transfer the solution to HB-Line for purification by anion exchange. Anion exchange will be followed by plutonium(IV) oxalate precipitation, filtration, and calcination to form PuO 2. The filtrate solutions, remaining after precipitation, contain low levels of Pu ions, oxalate ions, and may include solids. These solutions are transferred to H-Canyon for disposition. To mitigate the criticality concern of Pu solids in a Canyon tank, past processes have used oxalate destruction or have pre-filled the Canyon tank with a neutron poison. The installation of a filter on the process lines from the HB-Line filtrate tanks to H-Canyon Tank 9.6 is proposed to remove plutonium oxalate solids. This report describes SRNL's efforts to determine the appropriate pore size for the filters needed to perform this function. Information provided in this report aids in developing the control strategies for solids in the process. The tests performed during this effort report the following results.  Percent losses to the filtrate were < 1% for four of five tests and 1.5% for one test.  Sub-micron particle sizes are retained by initial filtration using a 10 μm filter. The filter cake aids in the filtration of the smaller particles.  The mean particle size increases with an increase in the initial acid concentration.  Larger mean particle sizes were observed when changing from a nitric acid/oxalic acid flush to nitric acid alone.  The size of Pu oxalate particles in HB-Line filtrate solutions averages 2.0 ± 0.4 μm in range of precipitation conditions tested. Further development of the "filter the filtrate" strategy must be geared to retain particles of the 2 μm size range.

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Section: Methodsmentioning

confidence: 99%

Section: Precipitation and Filtration Of Plutonium Oxalatementioning

confidence: 99%

Section: Particle Size Analysismentioning

confidence: 99%

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Determination of filter pore size for use in HB line phase II production of plutonium oxide

Shehee

Crowder

Rudisill

2014

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“…2 The samples evaluated in this report were purified PuO 2 samples produced from a variety of Pu(IV) oxalate precipitation and calcination conditions as part of AFS-2 development activities. 3 For perspective, the standard specification limit 1 for C content in AFS-2 oxide is 1000 g/g Pu, and the desired specification limit 4 for AFS-2 oxide is 500 g C/g Pu.…”

Section: Introductionmentioning

confidence: 99%

Initial Development of a Method to Measure Carbon by Thermogravimetric Analysis-Mass Spectrometry

Duffey¹

2014

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“…In addition, a series of small Pu(IV) oxalate precipitation tests with different digestion times were conducted to better understand the effect of digestion time on particle size, filtration efficiency and other factors. 4 To test the recommended process conditions, researchers performed two nearly-identical largerscale precipitation and calcination tests. The calcined batches of PuO 2 were characterized for density, specific surface area (SSA), particle size, moisture content, and impurities.…”

Section: Introductionmentioning

confidence: 99%

Lab-Scale Demonstration of Plutonium Purification by Anion Exchange, Plutonium (Iv) Oxalate Precipitation, and Calcination to Plutonium Oxide to Support the Mox Feed Mission

Small-Scale Testing of Plutonium (Iv) Oxalate Precipitation and Calcination to Plutonium Oxide to Support the Mox Feed Mission

Cited by 10 publications

References 2 publications

Determination of filter pore size for use in HB line phase II production of plutonium oxide

Determination of filter pore size for use in HB line phase II production of plutonium oxide

Initial Development of a Method to Measure Carbon by Thermogravimetric Analysis-Mass Spectrometry

Lab-Scale Demonstration of Plutonium Purification by Anion Exchange, Plutonium (Iv) Oxalate Precipitation, and Calcination to Plutonium Oxide to Support the Mox Feed Mission

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