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Title: Results of Characterization and Retrieval Testing on Tank 241-C-110 Heel Solids

Nine samples of heel solids from tank 241-C-110 were delivered to the 222-S Laboratory for characterization and dissolution testing. After being drained thoroughly, the sample solids were primarily white to light-brown with minor dark-colored inclusions. The maximum dimension of the majority of the solids was <2 mm; however, numerous pieces of aggregate, microcrystalline, and crystalline solids with maximum dimensions ranging from 5-70 mm were observed. In general, the larger pieces of aggregate solids were strongly cemented. Natrophosphate [Na{sub 7}F(PO{sub 4}){sub 2}°19H{sub 2}O] was the dominant solid phase identified in the heel solids. Results of chemical analyses suggested that 85-87 wt% of the heel solids were the fluoridephosphate double salt. The average bulk density measured for the heel solids was 1.689 g/mL; the reference density of natrophosphate is 1.71 g/mL. Dissolution tests on composite samples indicate that 94 to 97 wt% of the tank 241-C-110 heel solids can be retrieved by dissolution in water. Dissolution and recovery of the soluble components in 1 kg (0.59 L) of the heel solids required the addition of &#8776;9.5 kg (9.5 L) of water at 15 °C and &#8776;4.4 kg (4.45 L) of water at 45 °C. Calculations performed using the Environmental Simulation Program indicatemore » that dissolution of the &#8776;0.86 kg of natrophosphate in each kilogram of the tank 241-C-110 heel solids would require &#8776;9.45 kg of water at 15 °C and &#8776;4.25 kg of water at 45 °C. The slightly larger quantities of water determined to be required to retrieve the soluble components in 1 kg of the heel solids are consistent with that required for the dissolution of solids composed mainly of natrophosphate with a major portion of the balance consisting of highly soluble sodium salts. At least 98% of the structural water, soluble phosphate, sodium, fluoride, nitrate, carbonate, nitrite, sulfate, oxalate, and chloride in the test composites was dissolved and recovered in the dissolution tests. Most of the {sup 99}Tc and {sup 137}Cs present in the initial heel solids composites was removed in the water dissolution tests. The estimated activities/weights of {sup 129}I, {sup 234}U, {sup 235}U, {sup 236}U, and {sup 238}U in the dry residual solids were <25% of the weights/activities in the initial composite solids. Gibbsite and nordstrandite [both Al(OH){sub 3}] were the major solid phases identified in the solids remaining after completion of the dissolution tests. Chemical analysis indicated that the residual solids may have contained up to 62 wt% Al(OH){sub 3}. Significant quantities of unidentified phosphate-, iron-, bismuth-, silicon-, and strontium- bearing species were also present in the residual solids. The reference density of gibbsite (and nordstrandite) is 2.42 g/mL. The measured density of the residual solids, 2.65 g/mL, would be a reasonable value for solids containing gibbsite as the major component with minor quantities of other, higher density solids. Sieve analysis indicated that 22.2 wt% of the residual solids were discrete particles >710 &#956;m in size, and 77.8 wt% were particulates <710 &#956;m in size. Light-scattering measurements suggested that nearly all of the <710-&#956;m particulates with diameters >12 &#956;m were weakly bound aggregates of particles with diameters <2 &#956;m. The <710-&#956;m residual solids settled very slowly when dispersed in reagent water. The physical appearance of a suspension containing &#8776;0.4 vol% of the solids in pure water changed very little over a period of 46.5 hours. It should be noted that the distribution of particle sizes in the residual solids and the observed settling behavior were both strongly influenced by the procedures followed in the dissolution tests.« less
Publication Date:
OSTI Identifier:
Report Number(s):
LAB-RPT-13-00001 Rev 0
DOE Contract Number:
Resource Type:
Technical Report
Research Org:
HNF (Hanford Site (HNF), Richland, WA (United States))
Sponsoring Org:
USDOE Office of Environmental Management (EM)
Country of Publication:
United States