Sludge Batch (Decant No. 5) Frit 202 Flowsheet Demonstration Page: 17 of 39
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Immobilization Technology Section WSRC-TR-2003-00138
Savannah River Technology Center Rev. 0
Westinghouse Savannah River Company
4.0 DISCUSSION
4.1 FEED PREPARATION (22-L GLASS SRAT/SME RUNS)
Each SRAT/SME run at ACTL began with -16,000 grams of SB3 (Decant #5) sludge simulant
(Lorier 2003). An air purge and helium purge, as appropriate, were added to the kettles at
flowrates of -3372 seem and 16.9 secm, respectively. Nominal amounts of sieved coal, sand, and
trim chemicals - silver nitrate, gadolinium nitrate, palladium nitrate hydrate, rhodium nitrate
dihydrate, and ruthenium chloride, were then added. The addition of 33 ml of antifoam (IIT 747,
10%) was also performed prior to heating the vessels to 930C for acid addition. Once 930C was
achieved, nitric acid was first added to the vessel, followed by formic acid. Upon completion of
the acid addition, the mantle temperature setpoint was increased to 1100C for boiling, and 66 ml
of antifoam were added. The batch was then dewatered (concentrated to original volume), and
then refluxed for 12 hours after dewatering was completed. The SRAT cycles were complete
after this point, and the SME cycles were immediately begun.
At the beginning of the SME cycles, the air purge of each kettle was lowered to -1184 secm, the
helium purge lowered to 6.0 seem as appropriate, and 16.5 ml of antifoam were added to each
kettle. The temperature was lowered to -930C for the first frit addition. The first frit addition
was performed by adding the amounts of Frit 202, formic acid, and deionized water, specified in
the run plan. The contents of the kettle were heated again to boiling for dewatering /
concentration. The second frit addition proceeded in the same manner as the first. With both frit
additions, the target final feed material waste loading was 35%. Upon completion of the final
concentration addition, the contents of the kettle were cooled and then transferred into a carboy -
all final SME products were transferred into the same carboy for batch consistency.
The pH was monitored throughout the runs. Figure 4-1 displays the measured pH for the four
runs. All runs were similar in behavior. Some offset of pH is seen during the SME cycles
depending on the length of time required to complete the dewatering / concentration with each frit
addition. All of the SRAT and SME products had a measured pH of >7 at the elevated
temperatures.7
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Smith, M.E. Sludge Batch (Decant No. 5) Frit 202 Flowsheet Demonstration, report, June 2, 2003; South Carolina. (https://digital.library.unt.edu/ark:/67531/metadc736900/m1/17/: accessed April 17, 2024), University of North Texas Libraries, UNT Digital Library, https://digital.library.unt.edu; crediting UNT Libraries Government Documents Department.