Argonne National Laboratory has developed an electrometallurgical treatment for DOE spent metallic nuclear fuel. Fission products are immobilized in a durable glass bonded sodalite ceramic waste form (CWF) suitable for long term storage in a geological repository. Cesium is estimated to be in the waste form at approximately 0.1 wt.%. The exact disposition of cesium was uncertain and it was believed to be uniformly distributed throughout the waste form. A correlation of X-ray diffractometry (XRD), electron microscopy (EM), and nuclear magnetic resonance spectroscopy (NMR) performed on surrogate ceramic waste forms with high cesium loadings found a high cesium content in the glass phase and in several non-sodalite aluminosilicate phases. Cesium was not detected in the sodalite phase.
Interactions between the glass and crystalline phases of ceramic waste forms were investigated via powder X‐ray diffraction, scanning electron microscopy, and 29Si, 27Al, 23Na, 7Li, and 35Cl magic angle spinning nuclear magnetic resonance spectroscopy. LiCl, NaCl, or KCl waste form samples were made with or without glass. The waste forms containing glass consist of sodalite and glass phases with minor amounts of nepheline. Samples without glass form varying amounts of sodalite and nepheline. The glass frit, intended to bind the zeolite particles together, changes in composition, showing marked increases in aluminum and alkali content.
The title compound, ∣Na6Li1.6K0.4Cl2∣[Al6Si6O24]‐SOD, is similar to sodalite proper, but the introduction of Li and K into the structure creates a reduction in unit-cell volume and additional collapse of the framework tetrahedra. Refinement of an X-ray powder diffraction pattern of a multiphase material yielded for sodalite a lattice parameter of 0.88427 (2) nm, an Al–O–Si bond angle of 137.9(3°), and Al–O and Si–O bond lengths of 0.1730(5) nm and 0.1620(5) nm, respectively. The angle of the unique Al–O–Si bond corresponds well with the 138° obtained by 29Si solid-state magic-angle-spinning nuclear magnetic resonance spectroscopy. This characterization is important since the compound constitutes an essential part of a radioactive waste form intended for a high-level waste repository.
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