Molten Salt Techniques

1. Introduction.- References.- 2. Actinides.- 1. Introduction.- 1.1. Perspective.- 1.2. Historical Availability of Actinides.- 1.3. Current Availability of Actinides.- 2. Special Enclosures Required for Actinides.- 2.1. Health and Safety Standards.- 2.2. Benchtop and Chemical Hood Enclosures.- 2.3. Glovebox Enclosures.- 2.4. Remote Handling.- 3. Materials Problems.- 3.1. Irradiation Degradation of Materials.- 3.2. Container Compatibility at High Temperatures.- 4. Microtechniques.- 5. Techniques for Purification of Multigram Quantities of Actinides and Their Salts.- 5.1. Aqueous Methods of Purification.- 5.2. Pyrochemical Preparative Chemistry.- 5.3. Final Steps of Purification.- 6. Metal Preparation and Purification.- 6.1. Reduction by Metal Vapor.- 6.2. Pressure Vessel or "Bomb" Reduction.- 6.3. Ambient Pressure Reduction of Actinide Salts.- 6.4. Pyrochemical Purification of Actinide Metals.- 7. Physical Properties Measurements.- 7.1. Melting Points and Phase Relationships.- 7.2. Other Physical Properties of Actinide Salts.- 8. Absorption Spectra.- 9. Electrochemistry.- 9.1. Conductance Measurements.- 9.2. Electromotive Force Measurements.- 10. Summary.- References.- 3. Cryolite Systems.- 1. Introduction.- 1.1. General.- 1.2. Physical Properties of Cryolite.- 1.3. Uses of Cryolite.- 2. Container Materials.- 2.1. Graphite.- 2.2. Boron Nitride.- 2.3. Metals.- 3. Preparative Techniques.- 3.1. Commercial Cryolite.- 3.2. Preparation of Aluminum Fluoride.- 3.3. Purification of Alkali Metal Fluorides.- 4. The Study of Thermodynamic and Physicochemical Properties.- 4.1. Vapor Pressure.- 4.2. Electrical Conductivity.- 4.3. Density.- 4.4. Surface Tension.- 4.5. Viscosity.- 5. Electrodes in Molten Cryolite.- 5.1. General.- 5.2. Gas Electrodes.- 5.3. Oxide Electrodes.- 5.4. Metal Electrodes.- 5.5. Conclusion.- 6. Spectroscopy in Molten Cryolite.- 6.1. General.- 6.2. The Windowless Cell.- 6.3. The Diamond-Windowed Cell.- 7. Miscellaneous Techniques.- 7.1. Removing Cryolite.- 7.2. Cryolite Mixtures.- 7.3. Laboratory Furnaces.- 8. Conclusion.- References.- 4. Reference Electrodes for Molten Electrolytes.- 1. Introduction.- 2. Theoretical Principles.- 2.1. Electrode Potentials and Potential Scales.- 2.2. Cell Types, Half-Cells, and Standard States.- 2.3. Significance of the Electrolyte-Junction Potentials.- 2.4. Types of Reference Electrodes.- 2.5. Special Features of Molten Salts and Their Importance for Molten-Salt Reference Electrodes.- 2.6. Standard Electromotive-Force Series of Molten Salts.- 3. Principles of Reference Electrode Construction and Application.- 3.1. Construction and Use of Molten Salt Reference Electrodes.- 3.2. Stability of Reference Electrodes.- 3.3. Interaction between Reference Electrode and Instrumentation.- 4. Description of Reference Electrodes.- 4.1. Chlorides, Bromides, Iodides.- 4.2. Chloroaluminates.- 4.3. Fluorides.- 4.4. Cryolites.- 4.5. Nitrates.- 4.6. Carbonates.- 4.7. Sulfates.- 4.8. Hydroxides.- References.- 5. Neutron Diffraction.- 1. Introduction.- 2. Molten Salt Structure.- 2.1. Structure Factors.- 2.2. Small-Angle Neutron Scattering (SANS).- 3. Neutron or X-Ray Diffraction.- 3.1. Combination of Neutron and X-Ray Data.- 3.2. Scattering Experiment.- 4. Samples Amenable to Neutron Diffraction Study.- 5. Sample Preparation.- 5.1. Isotope Exchange.- 5.2. Sample Drying.- 6. Sample Containers.- 7. Furnaces.- 8. Neutron Beam Facilities.- 8.1. Diffractometers.- 8.2. Experiment Time Scales.- 9. Data Analysis.- 9.1. Introduction.- 9.2. Magnetic Scattering.- 10. Melts Studied Using Neutron Diffraction.- 10.1. Melts of the Type MX.- 10.2. Melts of the Type MX2.- 10.3. Binary Melts.- 10.4. Melts Discussion.- 11. Summary.- References.- 6. Dry Boxes and Inert Atmosphere Techniques.- 1. Introduction.- 2. Equipment.- 2.1. Glove Bags.- 2.2. Glove Boxes.- 2.3. Transfer Ports for Enclosures.- 2.4. Gas Sources and Purification Systems.- 2.5. Accessories.- 3. Operation.- 3.1. Startup Procedures.- 3.2. Maintaining the Inert Atmosphere.- 3.3. Monitoring the Atmosphere.- 4. Common Operations Conducted inside Dry Boxes.- 4.1. Weighing and Volumetric Operations.- 4.2. Electrochemical Measurements.- 4.3. Spectroscopic Measurements.- References.