The Emission Spectrochemical Determination of Impurities in Plutonium

Technical Report · Tue Sep 01 04:00:00 EDT 1964

DOI:https://doi.org/10.2172/4005847· OSTI ID:4005847

Wenzel, A. W. ^[1]; Pietri, C. E. ^[1]

---

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

Quantitative emission spectrographic methods have been developed for the determination of impurities in plutonium using a spectrograph modified for gloved box operations. In one procedure, plutonium is separated from its impurities by adsorption on Dowex-1 anion-exchange resin in 8N HNO₃ to minimize spectral interference and health hazards. The impurity-rich effluent is analyzed under conditions developed for maximum sensitivity by excitation in a direct current arc using a gallium oxide matrix. Twenty-two elements (Ag, Al, Am, Ba, Be, Ca, Cd, Cr, Cs, Cu, Fe, K, Li, Mg, Mn, Mo, Na, Ni, Pb, Rb, V, and Zn) can be determined by this method. The average relative standard deviation of the method for densitometered elements is 15%. The lower limits of detection of the impurities compare favorably with those obtained by the carrier-distillation method and the cupferron-extraction method. The method has been used to analyze plutonium metal, plutonium sulfates, and plutonium nitrate solutions! it has been adapted to the analysis of dicesium plutonium hexachloride salts using a cesium chloride matrix; and it has been applied to plutonium-uranium compounds using a hydrochloric acid adsorption-elution scheme. The second procedure employs a cation-exchange resin, Dowex-50, for adsorption of plutonium in 0.2N HNO₃ allowing the impurities to pass into the effluent. The method is used to determine boron and silicon which cannot be adequately determined using the anion-exchange separation technique. Direct current arc techniques are used; boiler-cap electrodes and a sodium carbonate buffer afford optimum conditions for silicon determination while mannitol-complexing and an indium oxide matrix aid in the determination of boron. The average relative standard deviation for silicon is less than 9% while that for boron is within 12%.

• Research Organization: New Brunswick Laboratory (NBL), New Brunswick, NJ (United States)
• Sponsoring Organization: US Atomic Energy Commission (AEC)
• NSA Number: NSA-18-043377
• OSTI ID: 4005847
• Report Number(s): NBL--215
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
ALUMINUM
AMERICIUM
BARIUM
BERYLLIUM
CADMIUM
CALCIUM
CESIUM
CHROMIUM
COPPER
EMISSION
ERRORS
GLOVEBOXES
IMPURITIES
ION EXCHANGE
IRON
LEAD
LITHIUM
MAGNESIUM
MANGANESE
MOLYBDENUM
NICKEL
NITRIC ACID
PLUTONIUM
POTASSIUM
QUALITATIVE ANALYSIS
QUANTITATIVE ANALYSIS
RADIATION PROTECTION
REMOTE HANDLING
RUBIDIUM
SEPARATION PROCESSES
SILVER
SODIUM
SPECTROSCOPY
VANADIUM
ZINC