Semiannual Progress Report for the Period January 1961 through July 1961

Technical Report · Thu Mar 01 04:00:00 EST 1962

DOI:https://doi.org/10.2172/4785161· OSTI ID:4785161

Rodden, C. J. ^[1]

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

*Spectrophotometric Determination of Tin and Molybdenum with 8-Quinolinol* A procedure is presented for the determination of both molybdenum and tin in a -wide variety of samples with 8-quinolinol (oxine). The molybdenum complex is extracted with chloroform from a sulfate solution of the sample at pH O.85 and determined spectrophotometrically at 385 mp. The tin complex is then similarly extracted and determined after the addition of chloride to the sample solution. *Pyrohydrolytic Separation of Boron from Boron Minerals for Mass Spectro metric BH/B10 Ratio Determination* Boron is separated quantitatively from various boron minerals by pyrohydrolysis. The distillate is passed through a cation-exchange resin column to remove interfering strontium, rubidium, and other cations, after which the effluent is neutralized to pH 9"3 to an3- evaporated to dryness. The residue is suitable for the mass spectrometric determination of the Bn/B10 ratio. *Design and Construction of a Versatile Mass Spectrometer for the Isotopic Analyses of Gas, Liquid, and Solid Substances* A single-focusing mass spectrometer of 6-inch radius, 60° sector magnetic analyzer has been designed to analyze a wide range of sample materials that require high precision and accuracy in the low-mass range but which offers considerable flexibility to evaluate high-mass materials for comparison purposes. A gas, solid, or liquid type of analysis may be performed. A change-over can be made from one type of analysis to another with minimum loss of instrument time and requiring minimum technical knowledge. Single peak measurement, or ratio measurement may be made from M/e 6/7 to ^M/e 238/235, with the use of vibrating reed electrometers or an electron multiplier for measuring the ion beams. *The Stability of Plutonium Sulfate Tetrahydrate and Anhydrous Plutonium Sulfate* The stability of plutonium sulfate tetrahydrate and anhydrous plutonium sulfate has been evaluated. Recent tests disclose no significant change in the plutonium content of the tetrahydrate or the anhydrous salt for periods of at least 1.8 and 6 months, respectively. Both thermo gravimetry and chemical analysis showed the formula of anhydrous plutonium sulfate to be Pu(S0₄)2.000 ± 0.002. *The Stability and Stoichiometry of Dicesium Plutonium Hexachloride* Dicesium plutonium hexachloride has been prepared and its suitability as a primary standard for plutonium evaluated. The composition of the material has been determined by analysis and fits the formula Cs₂PuCl₆. Although the compound is stoichiometric^ it is susceptible to changes in relative humidities greater than 17% and showed a small but significant weight loss during a six-month testing period. *The Cation-Exchange Separation and Spectrographic Determination of Silicon in Plutonium* Silicon is separated from plutonium using a cation-exchange procedure prior to spectrographic determination. Plutonium(lll) in 0.2N nitric acid is adsorbed on Dowex-50 cation resin while silicon^ as silicate anion or colloid, passes unabsorbed into the effluent. The effluent is evaporated to dryness and the residue is dissolved in dilute nitric acid containing hydrofluoric acid. Aliquots of the solution are dried on graphite electrodes and excited in a D.C. arc. Typical results bn synthetic solutions give an estimated overall average deviation of ± 25% and sensitivities from 1 to 5 p.p.m. silicon. This method offers an alternate procedure to the carrier distillation technique which employs large amounts of plutonium dioxide as matrix for the determination of silicon in plutonium. *Spectrographic Determination of Trace Impurities in High-Purity Plutonium* The development of a sensitive method for the spectrographic determination of trace impurities in plutonium is continuing. The method was modified for use with plutonium sulfate samples, and enlarged to include the determination of boron, cadmium, and some alkali elements, and also for the estimation of americium. Plutonium breakthrough during the ion exchange separation of plutonium from its impurities was found to be < 0.001%. Data from plutonium metal analyzed at this laboratory generally agreed with results obtained on similar material at Hanford Atomic Products Operation. Methods were investigated for preparing high-purity reagents and reducing reference blank values in order to obtain greater sensitivity. At present seventeen elements may be determined in the 1st and 2nd optical orders using only 200 mg. of sample.

• Research Organization: New Brunswick Laboratory (NBL), New Brunswick, NJ (United States)
• Sponsoring Organization: US Atomic Energy Commission (AEC)
• NSA Number: NSA-16-014616
• OSTI ID: 4785161
• Report Number(s): NBL--177
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEAR CHEMISTRY
ACIDITY
BORON 10
BORON 11
BORON COMPOUNDS
DISTILLATION
EVAPORATION
MASS SPECTROMETERS
PYROLYSIS
QUANTITATIVE ANALYSIS
RESIDUES
RESINS
RUTHENIUM
SEPARATION PROCESSES
STRONTIUM