Semi-Annual Progress Report for the Period July 1959 through December 1959

Technical Report · Sun May 01 00:00:00 EDT 1960

DOI:https://doi.org/10.2172/4160968· OSTI ID:4160968

Eberle, A. R. ^[1]; Siddons, T. J. ^[1]; Wenzel, A. W. ^[1]; Kramer, H. ^[1]; Payne, E. C. ^[1]; Pietri, C. E. ^[1]; Nelson, Jr., L. C. ^[1]

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1. New Brunswick Laboratory (NBL), New Brunswick, NJ (United States)

Determination of Uranium(lll) in Magnesium Fluoride Slag: A tentative procedure for the determination of uranium(ill) in material containing uranium trifluoride, uranium metal, and uranium tetrafluoride by hydrogen evolution is described. The method is not applicable to materials such as magnesium fluoride slag which contain uranium oxides because of the oxidation of uranium(lll) by uranium(Vl). The reactivity of uranium trifluoride in hydrofluoric-hydrochloric acid was studied. Determination of Metallic Uranium in Black Oxide: A method is described for the determination of metallic uranium in black oxide by hydrogen evolution. The hydrogen liberated by the acid treatment of the black oxide is oxidized to water which is trapped by freezing. The collected water is determined by the Karl Fischer method. The quantity of water found is a measure of the metallic uranium present. Determination of Microgram Quantities of Uranium in Beryllium Metal: Microgram quantities of uranium are separated from beryllium by a tributyl phosphate (TBP) extraction procedure. The beryllium metal is dissolved in nitric and hydrochloric acids. The uranium, is extracted from the acid solution with TBP and then stripped from the TBP with hot carbonate solution. The amount of uranium in the final aqueous solution is determined fluorimetrieally. Spectrochemical Determination of Boron in High-Purity Graphltes: A rapid method is presented for the spectrochemical determination of boron in pure graphites. Boron results, with a precision of ± 10 per cent and an accuracy of about 20 per cent in comparison to chemical values, were obtained with a sieved graphite sample and CuF₂ as a carrier. The method in its present form, however, is not applicable to relatively impure graphites, cokes, and carbons. Determination of Uranium with High Precision: The high precision method for the determination of uranium is reported in detail. Reduction of uranium(iv) to uranium(ill) is carried out electrolytically by means of a solid amalgam-platinum electrode couple. The oxidation of uranium(lll) to uranium(lV) either by the reduction of the hydrogen ion or by the oxidation with surface air is followed potentiometrically with a solid amalgam-saturated calomel reference electrode. The titration is then completed by the addition of a slight excess of solid dichromate followed by a back titration with 0.01 N ferrous ammonium sulfate solution. The precision is greater than that obtainable by existing methods. In addition, a preliminary report on the separation of trace interfering elements from large amounts of uranium, either electrolytically or by solvent extraction, after cupferron precipitation, is presented. Thermal Stability Studies of U₃O₈: Studies on the composition of U₃O₈ derived from uranium peroxide and uranium oxalate under varying temperature conditions are described. Preparation and Study of Plutonium Sulfate Tetrahydrate for Use as a Primary Analytical Standard: Plutonium sulfate tetrahydrate has been prepared by evaporation of a dilute sulfuric acid solution of plutonium(lV). The material has been under study for 7 months to determine its suitability as a primary analytical standard of plutonium. The formula of the compound has been determined by analysis and is Pu(SO₄)₂•4H₂O. The composition of the material over a period of 5 to 7 months was not appreciably influenced by a fluctuating laboratory environment. It, also, was not appreciably affected by relative humidity in the range of 17 to 75 per cent. The plutonium content of the compound was found to be essentially unchanged during the testing period. Plutonium sulfate tetrahydrate was found to be stable up to a temperature of approximately 60 to 65°C. Ion Exchange Separation and Colorimetric Determination of Microgram Amounts of Iron in Plutonium: Microgram quantities of iron have been separated from plutonium by anion exchange and determined colorimetrically with ortho-phenanthroline. Plutonium(lV) and plutonium(Vl) are adsorbed on Dowex-1 anion resin in 8 N nitric acid while the unadsorbed iron(lll) is eluted. The effect of the interference of plutonium on the determination when the plutonium-iron ratio is 10⁴ to 1 was also studied. Determination of Uranlum-235 by Gamma Ray Spectrometry: A method is described for the determination of uranium-235 in a variety of uranium containing materials by means of gamma ray spectrometry. The method involves the use of a single channel pulse height analyzer and a gamma ray scintillation counter, for 2 ranges of isotopic content: 0.04 to 15 per cent and 15 to 95 Per cent uranium-235. The error of measurement at the 95 per cent confidence level for the higher uranium content range is ±0.5 per cent absolute. A comparison of values obtained by gamma ray spectrometry and those values obtained by mass spectrometry indicates a relative difference of ±3.6 per cent at the 95 per cent confidence level over the concentration range of 0.04 to 5.25 per cent uranlum-235 at the low uranium content range. Isotopic Abundance Measurements of Uranium with the Mass Spectrometer: The instrumentation and analytical technique used in the mass spectrometric determination of the isotopic abundance of uranium samples are briefly described.

• Research Organization: New Brunswick Laboratory (NBL), New Brunswick, NJ (United States)
• Sponsoring Organization: US Atomic Energy Commission (AEC)
• NSA Number: NSA-14-017811
• OSTI ID: 4160968
• Report Number(s): NBL-159
• Resource Relation: Other Information: Orig. Receipt Date: 31-DEC-60
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEAR CHEMISTRY
BERYLLIUM
COLOR
FLUORESCENCE
GAMMA SPECTROMETERS
GRAPHITE
HYDROGEN
INSTRUMENTS
ION EXCHANGE
IRON
MEASURED VALUES
METALS
PLUTONIUM SULFATES
PREPARATION
QUANTITATIVE ANALYSIS
SPECTRA
URANIUM
URANIUM 235
URANIUM FLUORIDES
URANIUM OXIDES
URANIUM TETRAFLUORIDE