SPECTROPHOTOMETRIC DETERMINATION OF MICRO QUANTITIES OF CHLORIDE IN PLUTONIUM METAL

Technical Report · Wed May 01 04:00:00 EDT 1963

OSTI ID:4639112

Bergstresser, K S

Micro quantities of chloride are determined spectrophotometrically after separation from plutonium metal by pyrohydrolysis. Complete separations are accomplished by heating samples of plutonium metal at 900 to 1000 deg C in a stream of argon initially saturated with water at 85 deg C. The gas stream sweeps the trace element, as hydrogen chloride, into an alkaline absorbing solution. Reagente are added to form colored ferric thiocyanate complex in an amount equivalent to the chloride, and concentration of the complex is determined spectrophotometrically as an indirect measurement of chloride. Optimum range of chloride concentration in analyzing 1-gram plutonium samples by this method is 10 to 50 ppm, with relative standard deviations of 12 and 8 percent, respectively. The range can be extended to 5 and 200 ppm by modifying sample size. Iodide, bromide, cyanide, and thiocyannte interfere in this spectrophotometric chloride method, but these ions normally are not present after a pyrohydrolytic separation. (auth)

• Research Organization: Los Alamos Scientific Lab., N. Mex.
• DOE Contract Number: W-7405-ENG-36
• NSA Number: NSA-17-035629
• OSTI ID: 4639112
• Report Number(s): LA-2921
• Country of Publication: United States
• Language: English

Related Subjects

ARGON
BROMIDES
CHEMISTRY
CHLORIDES
CYANIDES
ERRORS
HIGH TEMPERATURE
HYDROLYSIS
INTERFERING ELEMENTS
IODIDES
IRON COMPLEXES
ORGANIC SULFUR COMPOUNDS
PHOTOMETRY
PLUTONIUM
QUANTITATIVE ANALYSIS
SEPARATION PROCESSES
SPECTROSCOPY
TRACE AMOUNTS
WATER