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Chemical Processing Technology Quarterly Progress Report, April-June 1961

Description: The Idaho Chemical Processing Plant did not operate on fuel recovery during this period, due to extensive renovation and modiflcation of facilities. Potasslum fluoride was found to be an undesirable additive to the barium precipitating agent used in formation of barium fluozirconate, because of precipitation and loss of uranium, although essentially complete precipitation of zirconium was achieved. Addition of hydrofluoric acid with barium precipitant, to achieve a fluoride/zirconium mole ratio of 5.5, was found to give a total zirconium recovery of 05%, including approximately 10% recovered after concentration of the supernate from the original precipitation. Removal of 97% of the zirconium and fluoride from zirconium -uranium dissolver solutions was achieved by precipitation with two moles of sodium formate per mole of zirconium. Uranium was readily recovered from the concentrated filtrate and wash solution by TBP extraction. The preparation and characterization of zirconium nitrate dibutylphosphate are described, and the solubility in Amsco was found to be similar to that of the uranlum dibutylphosphate complex (2 to 4 x 10/sup -5/ M). Stability studies indicated very little, if any, oxidation of ferrous to ferric iron ln a normal raffinate environment, and ferrous iron has a very low molar extinction coefficsent (0.8) compared with that of uranium (15) in the spectral region near 415 m mu . Pilot plant studies of the fluidized-bed calcination process for reduction of radioactive liquld wastes to the more-easily-stored solid form was continued in the two-foot-square calciner with production, for the first time over a prolonged period of continuous operation, of alpha alumina-free product from a feed contalning substantial sodium. Intra-particle porosities ranging from 0.04 to 0.60 were obtained. Differences in alpha-forming tendency of amorphous aluminas with varied calcination histories were demonstrated but attempts at correlation with known variables in fluid bed calciner operation were not successful. Rapid ...
Date: November 10, 1961
Creator: Bower, J. R.
Partner: UNT Libraries Government Documents Department

CHEMICAL PROCESSING TECHNOLOGY QUARTERLY PROGRESS REPORT, JULY-SEPTEMBER 1962

Description: Aqueous zirconium fuel processing studies, directed at adapting the hydrofluoric acid process to continuous dissolution-complexing in order to increase the capacity of the ICPP process, resulted in two successful approaches to the complexing-feed adjustment step. Continuous in-line adjustment (conversion of uranium(IV) to uranium(VI) necessary for extraction) was accomplished in one minute or less at approximately 90 deg C; surges of dissolver product from the operating dissolver up to 1.9 times the flow sheet rate did not inhibit the oxidation of the uranium at this temperature. Batchwise mixing in air of dissolver product solution with complexer solution oxidized the uranium within two minutes at 23 deg C or higher. Further studies of continuous zirconium dissolution indicated that precipitation of uranium at the acid inlet can be a problem, probably because of local concentration gradients of free HF, which result in conditions of low uranium solubility. Control of dissolver acid composition by electrical conductance measurement appeared possible due to the linear relationship of conductance with acid concentration. Aluminum alloy dissolution rates in nitric acid were found to vary significantly, depending on the type and amount of alloying agent. Silicon, nickel, and copper in the alloy significantly decreased the dissolution rate. Batch dissolution times for standard test coupons ranged from 14 minutes for a high purity aluminum to 1400 minutes for an alloy containing 2.9 percent silicon. In the electrolytic dissolution of Nichrome in a bench-scale basket dissolver, the substitution of titanium for niobium as the anode basket material significantly reduced the contact resistance. Current interruption due to contact failure was essentially eliminated, and contact resistance on the titanium was sufficiently low that increasing solution resistance due to acid depletion became a major contributor to current decline as dissolution progressed. The indirect solution-contact electrolytic dissolution principle was further studied, producing data on electrode ...
Date: December 28, 1962
Creator: Bower, J.R. ed.
Partner: UNT Libraries Government Documents Department

Chemical Processing Technology Quarterly Progress Report, April-June 1962

Description: Aqueous zirconium fuel processing studies, directed at adapting the hydrofluoric acid process to continuous dissolution-complexing in order to increase the capacity of the ICPP process, resulted in determination of dissolution rates over a wide range of conditions. The addition of oxidants to 4.8M hydrofluoric acid used for the continuous dissolution of 3% uranium-Zircaloy- 2 fuel decreased the amount of uranium-containing residue in the dissolver at the expense of a decreased dissolution rate. Oxidized fuel was dissolved in 4.8M hydrofluoric acid by use of heat to initiate the reaction: the oxide film remained behind as a dissolver residue. Uranium in the dissolver product was oxidized to the extractable form by one minute treatment at 92 deg C with aluminum nitrate complexer solution: only 59% was extractable after 24-hour treatment at room temperature. Several hundred hours operation of a continuous bench scale unit indicated that uranium buildup should not be a problem in the dissolver since an apparent equilibrium was soon established. After 650 hours of operation, a Monel dissolver showed some signs of localized corrosion but exhibited generally good resistance. Preliminary results in a study of aluminum alloy dissolution rates, initiated because of unusually slow dissolution of certain aluminum-based fuel elements, showed that nickel and copper ions in solution significantly retarded the dissolution rate while iron had an accelerating effect. Examination of specimens from the permanent ICPP raffinate storage tanks for aluminum process wastes indicated negligibie corrosion to date. Electrolytic dissolution studies progressed to a bench scale basket-type dissolver operating at currents up to 500 amperes with Nichrome fuel. Sudden current failures were essentially eliminated by use of platinum liners and a canted dissolver basket, but sustained operation was not attained because of a gradual decline in current as dissolution caused recession of the contact points on the dissolving rods. An ...
Date: September 24, 1962
Creator: Bower, J. R.
Partner: UNT Libraries Government Documents Department

Chemical Processing Technology Quarterly Progress Report, January-March 1961

Description: Studies are reported on aqueous zirconium processing, dissolution of BeO- UO/sub 2/ ceramic fuel, the aqueous stainless steel process, the behavior of dibutyl phosphates, use of boron (boric acid) solution to assure critical safety, fluidized bed calcination, conversion of amorphous alumina to alpha alumina, the Demonstrational Waste Calcining Facility, removal of long-lived radioisotopes from waste solutions, separation of iron, nickel, and chromiun from stainless steel waste solutions, electrolytic dissolution, effects of stray currents, electrolytic disintegration of Zircaloy-2, corrosion evaluation of materials of construction, the ARCO process, a direct air pulsed extraction column, and large vessel criticality control. (M.C.G.)
Date: October 31, 1962
Creator: Bower, J. R.
Partner: UNT Libraries Government Documents Department

Chemical Processing Technology Quarterly Progress Report, January-March 1962

Description: The processing of Al fuel, principally of the MTR-ETR type, is reported. Processing rate averaged 90% of flow sheet values for the entire operating period, and a U recovery of 99.85% was achieved. Aqueous Zr fuel processing studles continued with the objective of adapting the HF process to continuous dissolution-complexing in order to increase the capacity of the ICPP process while using as much existing equipment as possible to minimize costs. Good results were indicated in a 190-hr run dissolving 2% U-Zr fuel in a Monel dissolver using 4.8M HF-0.03M HNO/sub 3/ dissolvent at 200 deg F; insoluble material did not accumulate in the dissolver, although a U-containing film was formed, apparently in small, equilibrium quantity. Shorter term continuous laboratory dissolutions indicated that 4.8M acid was preferable to 10M acid for the acid feed rate/fuel surface ratios proposed, resulting in dissolver products of greater stability and higher uranium content. Additional laboratory data are presented on UF/sub 4/ hydrate form and solubility, together with maximum dissolvable U compositions with Zircaloy under various flowsheet condltions. Processing of Al alloys containing high Si was found to present no unusual problems in laboratory studies. Siliceous residues resulting from dissolution of Al-U alloys containing 2% Si in HNO/sub 3/ contained no insoluble U, and the occluded U was readily removed by solvent extraction with TBP-Amsco, the normal process extractant. Studies of the electrolytic dissolution process were directed at corrosion measurement and prevention, development of analytical systems for process control, and testing of structural insulating materials for use in the process environment. A measurement of corrosion potential is shown to indicate the instantaneous corrosion rate of stainless steel process equipment containing electrolytic dissolver solutions; this measurement could determine the amount of cathodic protection that might be used to protect certain corrosion sensitive areas. An in-line process ...
Date: June 29, 1962
Creator: Bower, J. R.
Partner: UNT Libraries Government Documents Department

Chemical Processing Technology Quarterly Progress Report, July-September 1961

Description: The Idaho Chemical Processing Plant did not operate on fuel recovery during the period since numerous repairs and modifications were being made to the extraction and U concentration equipment, Ba/sup 140/ production continued on schedule; substantial decontamination of the RaLa facility was achieved and desirable replacement or repair of in-cell equipment was accomplished in the interval between two successive runs. Aqueous Zr fuel processing studies continued with the obje tive of adapting the HF process to continuous dissolution a complexing in order to increase the capacity of the ICPP process while using as much existing equipment as possible to minimize costs. Dissolution rates for Zircaloy-2 in 10M(bar) fluoride dissolver solution proved to be adequate for continuous dissolution (as high as 79 mg cm/sup -2/ min/sup -1/) in an acid range which resulted in both controlled gas evolution and stable dissolver solutions. Preliminary results indicate the possibility of blending Zr raffinates from this process with larger volumes of Al raffinates to achieve stable waste solutions and avoid the necessity of constructing additional special alloy tanks for Zr waste. Supplemental studies on the sodium formate process for head end precipitation of Zr snd fluoride are reported, as well as results of corrosion tests on materials of construction considered for use in various zirconium processing applications. Other aqueous processing studies included the determination that 2.2M aluminum nitrate solutions, acid deficient to 1.0N/sup b/, could be used to scrub highly acid U extraction solutions without incurring the hazard of ammonium diuranate precipitation. Preliminary to processing organic moderated reactor fuel elements, it was discovered that carbonaceous films present on some elements were resistant to removal by Turco 4502 solution, and responded only to oxidation at 500 deg C; the possibility of processing without film removal was explored with satisfactory results insofar as dissolution of the ...
Date: December 18, 1961
Creator: Bower, J. R.
Partner: UNT Libraries Government Documents Department

Chemical Processing Technology Quarterly Progress Report, October-December 1960

Description: ICPP Operations. Changes made in processing equipment are described, and the use of continuous steam stripping to free waste solvent of Pu is described. Agueous Processing Studies. Studies were made of methods for separating Zr from dissolver solutions of U-Zr alloys. Recovery of U from BeO/ sub 2/-UO/sub 2/ ceramic fuels by grinding-leaching technique using boiling HNO/ sub 3/ reached 75 to 80%. Waste Calcination. Test results of feed spray nozzles for use in the Demonstrational Waste Calcining Facility are given. Studies were made on the calcination of aluminum nitrate and zirconium fluoride waste solutions. Waste Treatment. Removal of Cs and Sr from wastes by adsorption was investigated. The conditions for optimum separation of Fe, Ni, and Cr by Hg cathode electrolysis from waste solutions resulting from processing of stainless steel reactor fuels were determined. Electrolytic Dissolution Systems. The electrolytic dissolution of type 304 stainless steel was studied in the transpassive region as a function of electrode potential and HNO/sub 3/ concentration. An analog simulation study of an electrolytic dissolver is described. A niobium cathode in an electrolytic dissolver dissolving stainless steel in boiling HNO/sub 3/ did not absorb H/sub 2/. The corrosion resistance of several container materials to 1 M HNO/sub 3/ solution containing stainless steel was measured. Electrolytic disintegration of Zircaloy-2 in HNO/sub 3/ was studied. ARCO Process. The ARCO process was adapted to dissolutiom of UO/sub 2/ by addition of Cu as a catalyst to the PbCl/sub 2/-Cl/sub 2/ system. Dissolution rates were measured for Nb in molten PbCl/sub 2/. Equipment Development. Equipment for air pulsing of extraction columns and for preventing criticality of enriched U solutions are described. (D.L.C.)
Date: May 15, 1961
Creator: Bower, J. R.
Partner: UNT Libraries Government Documents Department

Chemical Processing Technology Quarterly Progress Report, October-December 1961

Description: The ICPP processed Al fuel, prtncipally of the MTR-ETR type, durtng this quarter. Newly designed and installed processing equipment exhibited excellent operating performance. This included direct-air-pulsed extraction, stripping and scrub columns, and a cascade-controlled continuous evaporator in first cycle product concentration service. Aqueous zirconium fuel processing studies continued with the objective of adapting the hydrofluoric acid process to continuous dissolution-complexing to increase the capacity of the LCPP process while using as much existing equipment as possible to minimize costs. Six variations of hydrofluoric acid flowsheets were tested in a smallscale continuous dissolvers. Dissolution rates were found to be high in all cases and dissolution was easily initiated at temperatures as low as 36 deg C. Monel and Carpenter 2O(Nb) were found to be satisfactory construction materials, from the standpoint of corroston, if oxidizing conditions were carefully controlled. Additional studies are reported on the stability of blended Zr and Al process raffinates and on the nature of the solids which result from the sodium formate headend precipitation process. Electrolytic dissolution studies, dtrected at fundamentals of current utiltzation in a series''-type dissolver, demonstrated that high current utilization is obtained when the polarization resistance is small compared with the solution resistance. Factors affecting polarization resistance and solution resistance are clarifted. A decrease in current utilization observed with alternating current as compared with direct current may be offset by efficiencies in elimination of a-c-d-c converters required for the d- c system. Experimental results indicate the possible usefulness of several plastic and ceramic materials tn the chemical and radiation environment of an electrolytic dissolver. Fluidized bed calcination tests conducted in pilot plant and demonstrational waste calcination facility calciners demonstrated that alpha alumina formation was suppressed by addition of boric acid to the waste aluminum nitrate feed. A possible relationship between nozzle design and alpha alumina ...
Date: March 28, 1962
Creator: Bower, J. R.
Partner: UNT Libraries Government Documents Department

IDAHO CHEMICAL PROCESSING PLANT TECHNICAL PROGRESS REPORT FOR JANUARY- MARCH 1960

Description: 9 > ? ( ing schedule included MTR, ETR, and other aluminum-type fuels that were processed through the TBP headend at 75 to 100% of flowsheet rates and through the Hexone second and third cycle extraction system at up to l5O% of flowsheet values, achieving an over-all recovery of 99.60%. In carrying out basic studies on aqueous zirconium processing, results obtained during the potentiometric titration of zirconium-fluoride-nitric acid solutions with sodium hydroxide were explained by a mechanism in which the untitrated zirconium fluoride species is converted to a fluozirconate and further hydrolysis proceeds via a fluozirconate route. A modified Zirflex flowsheet for processing 2.5% U-Zr alloy fuels is proposed as a result of bench scale dissolution studies on unirradiated PWR plates that showed that dissolver solutions could be stabilized by adding aluminum nitrate and nitric acid. that higher ammonium fluoride concentrations increased the dissolution rate, that higher hydrogen peroxide concentrations lowered the dissolution rate and decreased solution stability, and that ammonia removal by boiling with or without air sparging had little effect on the reaction. Density curves for Zirflex solutions are reported. First tests of the pilot plant for continuous dissolution of zirconium-type elements have indicated that the dissolution rate is approximately four times as great as predicted on the basis of batch dissolution rates and comparison with the rate ratio for batch vs. continuous dissolution of aluminum, which was used to establish the dissolver size. The continuous dissolution rate for a 2% zirconium- 98% uranium element was approximately proportional to the acid feed rate and reached l9O kg/day at an acid feed rate of 36 l/hr (11M nitric acid, 0.30M hydrofluoric acid, and 0.35M aluminum nitrate). Development of new waste treatment methods is influenced by waste volumes and the associated storage costs involved. A survey of current and proposed ...
Date: July 13, 1960
Creator: Slansky, C.M.; Warzel, F.M. & Bower, J.R. Jr. ed.
Partner: UNT Libraries Government Documents Department

Assessment of strength limiting flaws in ceramic heat exchanger components. Final report, September 1984--June 1993

Description: The ability to predict energy efficient lifetimes for ceramic heat exchanger components is necessary for their design, manufacture, and sale. The ability to inspect components for critical defects and adherence to specifications is also vital. This is the final report of a three phase program. In phase 1, various nondestructive evaluation methods were evaluated for use on siliconized silicon carbide heat exchanger tubes. The more promising ones were further developed for use in phase 2. These methods were used to examine samples used in a mechanical testing program, carried out at room temperature and at high temperature, to determine the detectability of defects and the effects of load at high temperature. A model was developed for fast fracture reliability. During phase 3, the equipment installed during phase 2 was modified for faster, easier ultrasonic scanning and microfocus X-ray computed tomography. This report describes the methods used to improve ultrasonic scanning of tubes, to reduce artifacts and enhance defect detection by X-ray computed tomography, to carry out pressure tests and high temperature C-ring tests with acoustic emission monitoring, and to generate a lifetime prediction model. The final model, the verification test results, and a general procedure for establishing specifications and acceptance tests for ceramics are presented.
Date: June 1, 1993
Creator: Bower, J.R.; Buttram, J.D.; Edwards, M.J.; Okes, L.R.; Powers, T.; Robertson, M.O. et al.
Partner: UNT Libraries Government Documents Department

ICPP Waste Calcining Facility : Safety Analysis Report

Description: Report documenting a study "made of the radiological hazards associated with operation of the ICPP Waste Calcination Facility" and contains "[d]etails of the safety analysis and extensive information on the process, equipment, and operation procedures" (p. iii). Each section has its own pagination.
Date: December 1, 1963
Creator: Lakey, L. T. & Bower, J. R.
Partner: UNT Libraries Government Documents Department

Silicon-Film{trademark} Solar Cells by a Flexible Manufacturing System

Description: AstroPower is developing a manufacturing process for Silicon-Film{trademark} solar cell production under the Photovoltaic Manufacturing Technology (PVMaT) cost-share program. This document reports on results from the first phase of a three-phase effort. Progress is reported on developing new procedures and equipment for in-line wet-chemical processes, metallization processes, sheet fabrication, solar cell processing, module assembly, solar cell testing, metallurgical-grade silicon purification, and recycling of Silicon-Film{trademark} sheet materials. Future concepts and goals for the Silicon-Film{trademark} process are also discussed.
Date: September 13, 1999
Creator: Culik, J. S.; Rand, J. A.; Bai, Y.; Bower, J. R.; Cummings, J. R.; Goncharovsky, I. et al.
Partner: UNT Libraries Government Documents Department