SUMMARYIdaho Nuclear Technology and Engineering Center 300,000-gallon vessel WM-189 was filled in late 2001 with concentrated sodium bearing waste (SBW). Three airlifted liquid samples and a steam jetted slurry sample were obtained for quantitative analysis and characterization of WM-189 liquid phase SBW and tank heel sludge. Estimates were provided for most of the reported data values, based on the greater of (a) analytical uncertainty, and (b) variation of analytical results between nominally similar samples.A consistency check on the data was performed by comparing the total mass of dissolved solids in the liquid, as measured gravimetrically from a dried sample, with the corresponding value obtained by summing the masses of cations and anions in the liquid, based on the reported analytical data. After reasonable adjustments to the nitrate and oxygen concentrations, satisfactory consistency between the two results was obtained. A similar consistency check was performed on the reported compositional data for sludge solids from the steam jetted sample.In addition to the compositional data, various other analyses were performed: particle size distribution was measured for the sludge solids, sludge settling tests were performed, and viscosity measurements were made.WM-189 characterization results were compared with those for WM-180, and other Tank Farm Facility tank characterization data.A 2-liter batch of WM-189 simulant was prepared and a clear, stable solution was obtained, based on a general procedure for mixing SBW simulant that was develop by Dr. Jerry Christian. This WM-189 SBW simulant is considered suitable for laboratory testing for process development. iv v ACKNOWLEDGEMENTS

Particle size distribution (PSD) analysis of radioactive slurry samples was obtained using a modified "off-the-shelf" classical laser light scattering particle size analyzer. A Horiba Instruments Inc. Model LA-300 PSD analyzer, which has a 0.1 to 600 micron measurement range, was modified for remote application in a "hot cell" (gamma radiation) environment. The general details of the modifications to this analyzer are presented in this paper.This technology provides rapid and simple PSD analysis, especially down in the fine and microscopic particle size regime. Particle size analysis of these radioactive slurries down in this smaller range was not achievable-making this technology far superior than the traditional methods used previously. Remote deployment and utilization of this technology is in an exploratory stage. The risk of malfunction in this radiation environment is countered by the gaining of this tremendously useful fundamental engineering data. Successful acquisition of this data, in conjunction with other characterization analyses, provides important information that can be used in the myriad of potential radioactive waste management alternatives.iv ACKNOWLEDGMENTS

SUMMARYDissolution kinetics of alumina type non-radioactive calcine was investigated as part of ongoing research that addresses permanent disposal of Idaho High Level Waste (HLW). Calcine waste was produced from the processing of nuclear fuel at the Idaho Nuclear Technology and Engineering Center (INTEC). Acidic radioactive raffinates were solidified at ~500ºC in a fluidized bed reactor to form the dry granular calcine material. Several Waste Management alternatives for the calcine are presented in the Idaho High Level Waste Draft EIS. The Separations Alternative addresses the processing of the calcine so that the HLW is ready for removal to a national geological repository by the year 2035. Calcine dissolution is the key front-end unit operation for the separations alternative.Because aluminum and zirconium-type fuels were predominately reprocessed at the INTEC, alumina and zirconia-type calcines were produced and stored. Dissolution kinetics testing with non-radioactive pilot plant zirconia calcine has been previously investigated. Similar to that work, the scope of this present alumina calcine dissolution work included: 1) chemical and physical analyses of the calcine material, 2) baseline dissolution testing to determine: order of reaction, activation energy (Arrhenius analysis), and dissolution rate controlling mechanism (chemical reaction or mass transfer limited). Testing was also performed to determine if complete dissolution is equilibrium/solubility inhibited.Chemical and physical analyses were performed on the RSH-1 alumina type pilot plant calcine bed material. Elemental fusion analysis results agree well with microprobe analysis results. An average value of the calcine acid consumption coefficient, b, was determined for RSH-1 bed product material; b = 19.8 grams RSH-1 dissolved per mol of acid consumed. The order of reaction testing revealed that, just as in the case for the Run74 zirconia pilot plant calcine testing, the homogeneous rate form fit the rate data better than the heterogeneous rate form. A characteristic dissolution fractal dimension, D R , was determined for alumina and zirconia pilot plant calcine milled material and bed particles. The result from this fractal treatment of the dissolution data further supports the indication that calcine dissolution is more dependent upon its physical characteristics, rather than its chemical characteristics. Arrhenius testing yielded an apparent activation energy (E A ) of 26.9 kcal/mol for RSH-1 alumina pilot plant calcine under conditions of constant 6 M acid concentration. The dissolution rate controlling mechanism testing results were inconclusive. Nevertheless, it was noted that, just as with all previous calcine dissolution testing, this testing with RSH-1 showed the familiar initial rapid dissolution then the leveling-out of the rate, and the non-attainment of 100% dissolution after long dissolution times-it too had the characteristics of internal mass diffusion controlled dissolution. The equilibrium/solubility inhibition testing results ind...

Particle size distribution (PSD) analysis of radioactive slurry samples was obtained using a modified "off-the-shelf" classical laser light scattering particle size analyzer. A Horiba Instruments Inc. Model LA-300 PSD analyzer, which has a 0.1 to 600 micron measurement range, was modified for remote application in a "hot cell" (gamma radiation) environment. The general details of the modifications to this analyzer are presented in this paper.This technology provides rapid and simple PSD analysis, especially down in the fine and microscopic particle size regime. Particle size analysis of these radioactive slurries down in this smaller range was not achievable-making this technology far superior than the traditional methods used previously. Remote deployment and utilization of this technology is in an exploratory stage. The risk of malfunction in this radiation environment is countered by the gaining of this tremendously useful fundamental engineering data. Successful acquisition of this data, in conjunction with other characterization analyses, provides important information that can be used in the myriad of potential radioactive waste management alternatives.iv ACKNOWLEDGMENTS

SUMMARYParticle size distribution (PSD) analysis of INTEC Tank Farm WM-182 and WM-183 heel slurry samples were performed using a modified Horiba LA-300 PSD analyzer at the RAL facility. There were two types of testing performed: typical PSD analysis, and settling rate testing.Although the heel slurry samples were obtained from two separate vessels, the particle size distribution results were quite similar. The slurry solids were from approximately a minimum particle size of 0.5 µm to a maximum of 230 µm-with about 90 % of the material between 2-to-133 µm, and the cumulative 50% value at approximately 20 µm. This testing also revealed that high frequency sonication with an ultrasonic element may break-up larger particles in the WM-182 and WM-183 tank farm heel slurries. This finding represents useful information regarding ultimate tank heel waste processing.Settling rate testing results were also fairly consistent with material from both vessels in that it appears that most of the mass of solids settle to an agglomerated, yet easily redispersed layer at the bottom. A dispersed and suspended material remained in the "clear" layer above the settled layer after about one-half an hour of settling time. This material had a statistical mode of approximately 5 µm and a maximum particle size of 30 µm.iv