Characterization of Tank 16H Annulus Samples

The closure of Tank 16H will require removal of material from the annulus of the tank. Samples from Tank 16H annulus were characterized and tested to provide information to evaluate various alternatives for removing the annulus waste. The analysis found all four annulus samples to be composed mainly of Si, Na, and Al and lesser amounts of other elements. The XRD data indicate quartz (SiO2) and sodium aluminum nitrate silicate hydrate (Na8(Al6Si6O24)(NO3)2.4H2O) as the predominant crystalline mineral phases in the samples. The XRD data also indicate the presence of crystalline sodium nitrate, sodium nitrite, gibbsite, hydrated sodium bicarbonate, and muscovite. Based on the weight of solids remaining at the end of the test, the water leaching test results indicate approximately 20-35% of the solids dissolved after three contacts with an approximately 3:1 volume of water at 45 C. The chemical analysis of the leachates and the XRD results of the remaining solids indicate sodium salts of nitrate, nitrite, sulfate, and possibly carbonate/bicarbonate make up the majority of the dissolved material. The majority of these salts were dissolved in the first water contact and simply diluted with each subsequent water contact. The water leaching removed large amounts of the uranium in two of the samples and ∼1/3 of the 99Tc from all four samples. Most of the other radionuclides analyzed showed low solubility in the water leaching test. The preliminary data on the oxalic acid leaching test indicate the three acid contacts at 45 C dissolved from ∼34-47% of the solids. The somewhat higher dissolution found in the oxalic acid leaching test versus the water leaching test might be offset by the tendency of the oxalic acid solutions to take on a gel-like consistency. The filtered solids left behind after three oxalic acid contacts were sticky and formed large clumps after drying. These two observations could indicate potential processing difficulties with solutions and solids from oxalic acid leaching. The gel formation might be avoided by using larger volumes of the acid. Further testing would be recommended before using oxalic acid to dissolve the Tank 16H annulus waste to ensure no processing difficulties are encountered in the full scale process.