This quarterly progress report discusses the ongoing work within the Solid State Division at the Oak Ridge National Laboratory for the period ending August 10, 1952. Projects discussed include radiation metallurgy, engineering properties, fused salts, crystal physics, and solid state reactions.

Abstract: A study was made of the reactions of nickel dipivaloyimethide with the following reagents: tirphenylmethyl chloride, benzoyl chloride, [rho]-chloro and [rho]-methyl benzoyl chloride. Infrared spectra of the easily hydrolyzed product of tritylation seem to indicate that enol ether, the product of O-alkylation, is formed. the acyl halides reactor to give the triketones. the latter have been characterized by spectra and C, H, analysis. the kinetics of all the reactions studied were found to settle down to a second order rate law after a fast initial reaction. These reactions are catalyzed by an impurity in the acyl chloride. Then benzoyl chloride with a different purity was used, the second order rate constant for the benzoylation of nickel DPM ranged from 0.02-0.20. The air oxidation of nickel dipivaloymethide was found to compete with the acylations under the conditions of these studies. An investigation of the phenomenon showed that nickel pivalate is the major product. Pivalic acid was also detected in the product mixture. This oxidation takes place in chlorobenzene and in aromatic hydrocarbons. It occurs in 1201 when small amount on benzoyl chlorides are present.

From Abstract: "A literature survey was made of both welding and brazing methods that might be used to minimize the amount of exposed core material and provide the longest path for corrosion in the event of a defective weld in enextruded Zircaloy-2-clad uranium and uranium-2 w/o zirconium fuel elements."

References to 193 publications of staff members of the Atomic Bomb Casualty Commission during 1947 through 1959 are listed in both English and Japanese. Author and subject indexes are included.

A report which compares the creep properties of 15 percent cold-worked zircaloy-2 and of annealed zircaloy-2 is being made.

"The factors of atomic size, ion core potential, and charge, which contribute to the increment in electrical resistivity produced by solutes in metallic solutions, were separated and experimentally evaluated in liquid sodium. The results are expressed in a semi-empirical relationship which defines the increment in resistivity of a monovalent solution as the sum of the fractional difference in atomic volume of solute and solvent and the difference in atomic number of Na and the solutes Li, K, Cs, Rb, Ag, and Au."

Abstract : Methods for the chemical separation of strontium, barium, cesium, cerium, yttrium, zirconium, niobium, and tungsten from complex matrices are described. Procedures for the radiometric determination of the longer-lived isotopes of these elements are outlined. Inert carriers are added and the sample is dissolved by fusion with sodium carbonate. The melt is leached first with water and then with hydrochloric acid. The elements are recovered from these fractions by a series of wet chemical and ion exchange procedures, and gravimetric and radiometric determinations performed.

Abstract: Both direct and coincidence counting apparatus are described. The elimination of cosmic ray events by coincidence plus gamma ray shielding permits the reduction of counting rates far beyond that obtainable with shielding alone. By selection of materials and development of new components and techniques, the residual background count of beta counting equipment can be reduced to a very low value. Geiger counter equipment for routine laboratory measurements is described, have a background count of 0.7 c/m. Scintillation counters are shown to have a background of 0.2 c/m at 30% efficiency. A portable Geiger counter with a 3.7 c/m background is also described.

Abstract: "Abnormally short interatomic distances are characteristic of aluminum-transition element compounds which occur at the aluminum-rich ends of the phase diagram." Summary: "The theoretical model assumed in this investigation was that of spherical distribution of electrons centered about atomic sites in the V4Al23 structure, represented by the theoretical scattering factors for the isolated atoms. ...It is evident from the (Fo-Fc)-synthesis maps that too much scattering power has been assumed in the immediate vicinity of each atomic site since the negative regions associated with these sties represent electron density differences which are generally two to three times greater than the estimated experimental errors. ...An estimate of the number of electrons associated with the positive regions in the (Fo-Fc)-synthesis maps, and presumably the number of electrons participating in the bonding, could be obtained by computing structure facts with theoretical scattering factors which account for the contributions of the core electrons only. An (Fo-Fc)-synthesis with these Fc values and the Fo values from this investigation should then approximate the actual distribution of the outer electrons."

From abstract: "The mass spectrum of stannane, SnH4, has been studied. Ion fragmentation patterns for both the singly and doubly charged fragments were obtained employing 70-volt electrons. From appearance potential data, an estimation of the bond energies of the tin-hydrogen bond in the ion-species SnH+3-H, SnH+2-H, SnH+-H, Sn+-H has been made along with [delta]Hf for SnH4. The studies were first made with tin of normal isotopic abundance, and then the results were corroborated with SnH4 prepared with the separated isotope 120Sn."

This report summarizes the hazards associated with the operation of the Lynchburg Test Reactor (LTR) critical experiments. The LTR critical experiment program is outlined and the design of the experiment is described. The experiments will provide basic data to check two-dimensional calculational methods and provide information needed in the design of the LTR.

This report provides an overview of the creation of the Liquid Metal Fuel Reactor Experiment program. It furthers the work by constructing a single loop to test all the components required for the 16 loop reactor. This utility loop was also constructed to provide a facility for testing various components such as valves and flow meters.

Technical report issued by E. I. du Pont de Nemours & Co. From Abstract: "Information obtained from investigations pertinent to tritium monitoring and protective measures at the Savannah River Plant are given. These findings were used to establish realistic protective techniques and consequently, to insure the safety of workers exposed to this hazard. Topics included are: contamination, permeation of plastics and rubber, instrumentation, and biological and physical aspects."

Technical report outlining experiments on aluminum-lithium alloys. From Abstract: "Aluminum-lithium alloys are subject to precipitation from solid solution, and may be age hardened by the same techniques used for more common aluminum alloys. Spherical particles of precipitate were observed with the electron microscope in 1.5% and 2.8% Al-Li alloys after aging for times comparable to those required to produce maximum hardness. Rod-shaped particles that were oriented parallel to either the (110) or the (111) planes of the aluminum matrix were observed in overaged specimens."

Technical report. From Abstract: "Precipitation of manganese dioxide in solutions of uranium-aluminum alloy effected maximum removal of fission products when the alloy solutions were acid deficient. Minimum adsorption of uranium and minimum volume of centrifuged MnO2 were obtained by precipitation in acidic solutions with vigorous agitation."

Technical report. From Abstract : "Ascorbic and isoascorbic acids, used in conjunction with sulfamic acid, reduced Pu(IV) rapidly and completely to Pu(III) in solutions of nitric acid. The solutions of Pu(III) were stable. Aminoguanidine sulfate also retarded the oxidation of Pu(III) but did not reduce Pu(IV)."

Technical report. From Abstract : "Predictions of the behavior of technetium in the Purex process and details of the chemistry of technetium for Purex process conditions are given."

Technical report. From Abstract: "An electromagnetical instrument is described which produces a shaft rotation which is a linear function of the quantity being measured from a non-linear input signal. The instrument was used to convert the output function of the Nuclear Test Gage (NTG) which is nonlinear with respect to fuel concentration to a form that will directly drive an automatic production recorder (APR). The output shaft is also geared to a Veeder Root counter so that the value of the independent variable is given to the NTG operator in digital form. A rate-of-change detector automatically trips the APR when the reading has come sufficiently close to equilibrium."

Technical report. From Abstract: "An ion exchange process was demonstrated for the recovery of Pu238 from irradiated neptunium oxide. Three cycles of anion exchange proved adequate for the removal of fission products and for the separation of the neptunium and plutonium from each other."

Technical report. From Abstract: "Ultrasonic energy appropriately applied to the die or container of a laboratory-type direct extrusion press effected a marked increase in the free extrusion rate of lead and aluminum billets at a constant extrusion rate. the same results were obtained in extrusion cladding steel tubes with aluminum. Rate increases were generally 100 per cent or greater, and decreases in force were usually within the range of 10 to 20 per cent. Furthermore, the shape and slope of the extrusion curves were altered. The effect appeared to be attributable to a reduction of both die friction and container wall friction under ultrasonic influence."

Technical report. From Abstract: "Rate data are presented for the oxidation of neptunium (V) by vanadium (V) in nitric acid." From Summary: "Rates of oxidation of neptunium (V) were determined by a solvent extraction technique based on the difference in distribution coefficients for neptunium (V) and neptunium (VI)."

Technical report. From Abstract: "A method of fastening thermocouples to 0.030-inch-thick aluminum cladding on test fuel elements was developed. The installation does not lead to hot spots by the addition of extra metal of the distortion of the cooling water channels. Fuel element temperatures were faithfully followed in SPERT tests up to the melting point. The method has been useful for fastening thermocouples to aluminum sections in general."

Preface: The intermediate heat exchanger is designed for operation in a nuclear power plant using liquid sodium as the primary and secondary coolant. Since the primary fluid coming from the reactor is radioactive, the purpose of the IHX is to transfer heat to a nonradioactive fluid which then goes to a steam generator. Because of this activity the until will be enclosed in a concrete pit and will not be accessible during periods of operation. Immediately after shut down it will be necessary to allow time for radioactive decay before the unit will be accessible to personnel. Because of inaccessibility and possible long periods allowed for decay time, it is imperative that the unit give trouble free operation. During periods of shut down, the internals should have easy access for inspection and repair if necessary so that down time is held to a minimum. The general arrangement of the heat exchanger described in this report presents a conventional design utilizing known materials and existing methods of fabrication. In further consideration of all concepts, designs and analyses developed during this period of the program, it is felt that this preliminary design will provide an intermediate sodium heat exchanger of lower cost …

Abstract: The caustic permanganate-rinse decontamination treatment was investigated. Loop and metallurgical studies were performed to determine optimum operating conditions as well as the metallurgical effects of the treatment. A treatment with 10 percent sodium hydroxide and 5 percent potassium permanganate solution followed by a rinse with a 5 percent ammonium citrate, 2 percent citric acid and 1/2 percent Versene solution was chosen for the decontamination of a stainless steel steam generator. Decontamination factors of greater than 50 were obtained in loop tests using the above treatment. Corrosion and metallurgical results indicated a total penetration of less than 0.01 mil on annealed Type 304 stainless steel with no evidence of any deleterious effects.