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Plutonium Speciation in Support of Oxidative-Leaching Demonstration Test

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Plutonium Speciation in Support of Oxidative-Leaching Demonstration Test PNNL-16844 WTP-RPT-165, Rev 0 Plutonium Speciation in Support of Oxidative­Leaching Demonstration Test S. I. Sinkov October 2007 Prepared for the U.S. Department of Energy under Contract DE-AC05-76RL01830 DISCLAIMER This report was prepared as an account of work sponsored by an agency of the United States Government. Neither the United States Government nor any agency thereof, nor Battelle Memorial Institute, nor any of their employees, makes any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or usefulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any specific commercial product, process, or service by trade name, trademark, manufacturer, or otherwise does not necessarily constitute or imply its endorsement, recommendation, or favoring by the United States Government or any agency thereof, or Battelle Memorial Institute. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or any agency thereof. PACIFIC NORTHWEST NATIONAL LABORATORY operated by BATTELLE for the UNITED STATES DEPARTMENT OF ENERGY under Contract DE-AC05-76RL01830 PNNL-16844 WTP-RPT-165, Rev 0 Plutonium Speciation in Support of Oxidative-Leaching Demonstration Test S. I. Sinkov October 2007 Test specification: 24590-PTF-TSP-RT-06-002, Rev 0. Test plan: TP-RPP-WTP-445 Test exceptions: none R&T focus area: Pretreatment Test scoping statements(s): None Pacific Northwest National Laboratory Richland, Washington 99352 3 Contents Abbreviation/Acronym List .......................................................................................................................xiii References................................................................................................................................................... xv Testing Summary....................................................................................................................................... xix Objectives........................................................................................................................................... xix Test Exceptions................................................................................................................................xxiii Results and Performance Against Success Criteria..........................................................................xxiii Quality Requirements....................................................................................................................... xxiv R&T Test Conditions ........................................................................................................................ xxv Simulant Use..................................................................................................................................... xxv Discrepancies and Follow-on Tests .................................................................................................. xxv 1.0 Introduction........................................................................................................................................ 1.1 1.1 Oxidation States and Redox Stability of Pu(IV, V, and V) in an Alkaline Medium.................. 1.2 1.2 Solubility of Pu(IV, V, and VI) in an Alkaline Medium............................................................ 1.3 1.3 Controversy in Determination of Stability Fields of Pu(IV), Pu(V), and Pu(VI) Soluble Species on Eh-pH Diagrams in Alkaline Solutions.................................................................... 1.5 1.4 Direct Speciation of Pu at Low Micromolar Concentrations by Spectroscopic Techniques ..... 1.8 1.5 Pu Solubilization and Speciation in the Process of Oxidative Alkaline Leaching of Hanford Tank Sludges.............................................................................................................. 1.10 1.6 The Project Goals..................................................................................................................... 1.10 1.7 Quality Assurance and Quality Control ................................................................................... 1.11 1.7.1 Application of RPP-WTP Quality Assurance Requirements......................................... 1.11 1.7.2 Conduct of Experimental and Analytical Work............................................................. 1.12 1.7.3 Internal Data Verification and Validation...................................................................... 1.12 2.0 Experimental and Data Processing..................................................................................................... 2.1 2.1 Reagents and Solvents Used in Calibration, Sludge Preparation, and Oxidative-Leaching Experiments................................................................................................................................ 2.1 2.2 The Preparation, Purification, and Valence-State Adjustment of Pu Stock Solutions ............... 2.1 2.3 Spectrophotometric Equipment.................................................................................................. 2.2 2.4 Calibration and Speciation Experiments with LWCC (cold testing and Pu calibrations).......... 2.3 2.5 Determination of Pu Concentration in Calibration Solutions and Leachates............................. 2.3 2.6 Preparation of the Fe(OH)3/Cr(OH)3/Pu(OH)4 Sludge Simulant and Oxidative-Leaching Procedure.................................................................................................................................... 2.4 v 2.7 Measurements of Eh and pH ...................................................................................................... 2.5 2.8 Determination of Cr(VI), Mn(VII), and Mn(VI) Concentrations in the Course of Oxidative-Leaching Experiments............................................................................................... 2.6 2.9 Baseline Subtraction and Net Peak Intensity Determination in Nd and Pu Calibration Experiments................................................................................................................................ 2.6 2.10 Simulation and Elimination of Waveform-Shaped Spectral Interference in LWCC Spectra Burdened with Low-Frequency Noise ....................................................................................... 2.6 3.0 Results and Discussion....................................................................................................................... 3.1 3.1 Light-Transmission Efficiency of LWCC.................................................................................. 3.1 3.2 Demonstration of Identity of Spectral Features of Nd(III) in H2O and D2O.............................. 3.4 3.3 Cold Testing of LWCC Using Nd(III) Complex with EDTA in 0.1 M NaOH and 0.1 M NaOD............................................................................................................................... 3.5 3.4 Pu(VI) Calibration and Speciation Experiments in DNO3 and NaOD....................................... 3.8 3.4.1 Pu(VI) Calibration Experiment in DNO3......................................................................... 3.8 3.4.2 Pu(VI) Calibration Experiments in NaOD..................................................................... 3.10 3.4.3 Pu(VI) Spectra in the Presence of Carbonate at Constant Concentration of Hydroxide ...................................................................................................................... 3.15 3.5 Pu(V) Calibration and Speciation Experiments in NaOD........................................................ 3.17 3.5.1 Preparation and Characterization of Pu(V) Solution in 14 M of NaOD........................ 3.17 3.5.2 Pu(V) Calibration and Speciation Experiments in NaOD ............................................. 3.20 3.5.3 Pu(V) Spectra in the Presence of Carbonate at Constant Concentration of Hydroxide ...................................................................................................................... 3.24 3.5.4 Pu(V) Redox Speciation After Acidification of Initially Alkaline Pu(V) Solution by DNO3 at a Low Micromolar Concentration of Pu(V)............................................... 3.29 3.5.5 Determination of Formal Electrochemical Potential of Pu(VI)/Pu(V) Couple in 0.25 M to 1.0 M NaOD Using Direct Potentiometric Measurement with an ORP Electrode ........................................................................................................................ 3.31 3.6 Pu(IV) Spectral Measurements in DNO3 and NaOD ............................................................... 3.32 3.6.1 Verification of Identity of Spectral Features of Pu(IV) in 4 M of HNO3 and 4 M of DNO3.................................................................................................................. 3.32 3.6.2 Pu(IV) Calibration Experiment in 0.75 M of DNO3 ...................................................... 3.34 3.6.3 Pu(IV) Speciation and Solubility in 0.25 M NaOD....................................................... 3.35 3.6.4 Pu(IV) Speciation and Solubility in 0.25 M NaOD in the Presence of Carbonate ........ 3.37 3.7 Oxidative Dissolution of Pu(IV) Hydroxide Suspension by Permanganate and Manganate in 0.25 M NaOD....................................................................................................................... 3.41 IV 3.7.1
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