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Title: SUMMARY TECHNICAL REPORT FOR THE PERIOD JULY 1, 1958 TO SEPTEMBER 30, 1958

Technical Report ·
OSTI ID:4136230

Stanleigh, Stanrock, Milliken, Dyno, and Rayrock concentrates were approved as feed materials for the Refinery. Ohio Oil Lignite--Northgate Lignite (a combined feed) has not been approved. The coalescence time of tributyl phosphate-kerosene solvent was reduced temporarily by treatment with activated bauxite. A relationship was found between the flooding capacity of an extraction column and the coalescence time of the solvent used. Electronic absorption spectral studies demonstrated that a stable, equimolar complex was formed in the tributyl phosphatenitric acid system between associated nitric acid (HNO/sub 3/) and tributyl phosphate (TBP). The addition of 750 ppm sulfate to ammoniated uranyl nitrate prior to pot denitration increased the reduction rate of the product UO/sub 3/. The addition of 750 ppm phosphate to sulfated uranyl nitrate prior to pot denitration slightly decreased the activating effect of the sulfate. Preliminary results are presented from the continuous diffraction study of the reduction of UO/sub 3/ to UO/sub 2/. The solids feed rate to a reduction reactor in the Green Salt Plant was controlled within plus or minus 2.5 per cent by a feed-control system. The reaction between steam and green salt to produce HF and UO/sub 2/ was demonstrated in the laboratory, utilizing thermobslance equipment. The reaction proceeds rapidly to completion at 1200 deg F and will yield aqueous HF containning at least 70 weight per cent HF at this temperature. A rectification column, seven feet high and one inch in ID was used to distill aqueous HF. The column was packed with 1/8-in. irregular carbon particles and was designed without a reboiler or stripping section for a saturated vapor feed. When a vapor feed of 66 per cent HF was used and the still was operated at total reflux, the distillate approached anhydrous HF, while the bottoms averaged 47.6 per cent HF. A vapor feed of 18 per cent HF resulted in a distillate of approximately 0.5 per cent HF and a bottoms concentration of 28.6 per cent HF. The results of brief scoping tests in the laboratory indicate the feasibility of a scheme for the recovery of anhydrous HF from depleted UF/sub 6/, based upon the following over-all chemical reaction: UF/sub 6/ + H/sub 2/SO/sub 4/ + 2 H/sub 2/O yields UO/sub 2/SO/sub 4/ + 6HF. The particle size distribution, morphological characteristics, and occurrence of contaminating phases were studied in samples of three types of green salt: standard, high-UO/sub 2/F/sub 2/, and high-AOI. In the pilotscale semi-cortinuous reduction of uranium tetralluoride to uranium metal, 6 per cent in excess of the stoichiometric amount of magnesium was found preferable to either 2 per cent or 4 per cent. A short-term reduction-pouring was demonstrated in a two-way tilt lip-pour induction furnace. Twenty-two reductions to uranium metal were performed in small-scale equipment, the average reduction conversion yield being 97.5 per cent. Tightly adhering slag was removed from 12-inch-diameter derbies by heating the derbies to 1300 to 1400 deg F and then quenching them in water. Graphite crucibles and graphite molds for the vacuum melting step were flame-sprayed with magnesium zirconate coating. The results of a statistically designed test indicated that there was no significant difference in the quality of the product produced at low and high pressure in a remelt furnace. The hydrogen pickup by uranium metal during heat treatment in 25 wt.% Li/sub 2/CO/sub 3/: 75 wt.% K/sub 2/CO/sub 3/ salt and in 50 wt.% HCl: 50 wt.% NaCl salt was compared. A recording flame photometer was used to identify the spectra of nine elements in typical uranium concentrates. A rapid spectrophotometric method for the determination of nitrate in orange oxide is described. The range of the TTA-Thoron method was extended to include the determi nation of one to ten ppm thorium in uranium metal. (For . preceding period see NLCO-750.) (W.L.H.)

Research Organization:
National Lead Co. of Ohio, Cincinnati
DOE Contract Number:
AT(30-1)-1156
NSA Number:
NSA-14-016695
OSTI ID:
4136230
Report Number(s):
NLCO-760
Resource Relation:
Other Information: Decl. Mar. 28, 1960. Orig. Receipt Date: 31-DEC-60
Country of Publication:
United States
Language:
English