In 1970, the Waste Management and Transportation Division of the Atomic Energy Commission ordered a segregation of transuianic (TRU)contaminated solid wastes. Those below a contamination level of 10 nCi/g could still be buried; those above had to be stored retrievably for 20yr. The possibility thet alpha-radiolysis of hydrogenous materials might produce toxic, corrosive, and flammable gases in retrievably stored waste prompted an investigation of gas identities and generation rates in the laboratory and field. Typical waste mixtures were synthesized and contaminated for laboratory experiments, and drums of actual TRU-contaminated waste were instrumented for field testing. Several levels of contamination were studied, as well as pressure, temperature, and moisture effects. G(gas) values were determined for various waste matrices, and degradation products were examined. Yes Yes Yes Yes Yes Yes Yes Yes Yes No Matrix
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Nitride nitrogen in B.C is determined by dissolving the sample in 14M H-SO, in a sealed fused-silica tube, distilling the nitrogen as ammonia from alkaline solution, and titrating the ammonium hydroxide in the distillation receiver with standardized acid. The Winkler distillation and the titration are proven operations that are directly applicable to the analysis of the B4C solution. Recovery of nitrogen from B4C was difficult and time-consuming by the usual caustic-fusion and leach methods, but it was simplified by substituting the technique of high-temperature dissolution in 14M HjSO*. With the sealed-tube method, analysis of six prepared mixtures of BN and B4C gave a mean recovery of 99.9% nitrogen, with a standard deviation of 0.94%. Fourteen portions of B^C production material gave a mean nitrogen value of 917 ppm, with a standard deviation of ± 30 ppm. Twelve analyses of tne same material by the caustic-fusion method gave a mean nitrogen content of 928 ppm, with a standard deviation of ± 84 ppm. The sealed-tube method for determining nitrogen is highly selective; nore of the impurities found in B4C interfere.
As part of a TRU waste-sampling program, Los Alamos National Laboratory retrieved and examined 44 drums of 238p u _ anf j 2 39p u-CO n tatnlna ted waste. The drums ranged in age from 8 months to 9 years. The majority of drums were tested for pressure, and gas samples withdrawn from the drums were analyzed by a mass spectrometer. Real-time radiography and visual examination were used to determine both void volumes and waste content. Drum walls were measured for deterioration, and selected drum contents were reassayed for comparison with original assays and WIPP criteria. Each drum tested at atmospheric pressure. Mass spectrometry revealed no problem with ^-^ Puc ontaminated waste, but three 3-month-old drums of 238p ucon taminated waste contained a potentially hazardous gas mixture. Void volumes fell within the 81-9 7% range. Measurements of drum walls showed no significant corrosion or deterioration. All reassayed contents were within WIPP waste acceptance cri terla. Five of the drums opened and examined (15%) could not be certified as packaged. Three contained free liquids, one had corrosive materials, and one had too much unstabilized particulate. Eleven drums had the wrong (or not the most appropriate) waste code. In many cases, disposal volumes had been inefficiently used.
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