THE SPECTROPHOTOMETRIC DETERMINATION OF ALLOYING AND FISSION PRODUCT ELEMENTS IN NONIRRADIATED PLUTONIUM 'FISSIUM' ALLOYS
In the development of fuel processing methods for purifying Pu--Fe or Pu- -Co fuel alloys, methods of chemical analysis were required for the alloylng element and representative fission-product elements. The initial plutonium fissium alloy, which represented 10% burn-up after 130 days of fast fission, contained 2.5% Co or -Fe, 0.7% Ce, 1.3% La, 0.7% Mo, 0.03% Nb, 1.3% Ru, and 0.8% Zr. The concentration of many of these elements was reduced in the fuel processing to less than 0.01%. It was necessary to devise chemical methods for determining each element in these concentration ranges except lanthanum, which was determined spectrographically. Dissolution of these alloys was accomplished by a sealed-tube technique, using HCI which contained a few drops of HCI0/sub 4/ as a solvent, or by heating the sample with HCI and HCI0/sub 4/ in a distillation apparatus until the ruthenium distilled as the tetroxide. Cerium was separated from Pu/sup 6+/ by precipitation of Ce/sup 4+/ fluoride, after which it was determined spectrophotometrically as Ce/sup 4+/. Cobalt was determined in the presence of plutonium by means of the color formed by cobalt in an HCI-acetone medium. Iron was determined by measuring the absorbancy of the ferrous-o- phenanthrolate complex, either in the presence of plutonium or after separation by extraction of FeCl/sub 3/. Molybdenum and zirconium were each determined colorimetrically as the chloranilates after separation of molybdenum by hexone extraction from HCI solution and precipitation of zirconium as the p- bromomandelate. Niobium was extracted into hexone from an H/sub 2/S0/sub 4/--HF medium and estimated by means of the color formed with hydroquinone in H/sub 2/SO/ sub 4/. Ruthenium was distilled as the tetroxide and estimated colorimetrically as Ru/sup 4+/ chloride. In the higher concentration ranges, the relative standard deviation for the determination of each element was less than 2%. At lower concentrations, relative standard deviations of 5% were acceptable. (auth)
- Research Organization:
- Los Alamos Scientific Lab., N. Mex.
- NSA Number:
- NSA-15-008756
- OSTI ID:
- 4102746
- Report Number(s):
- TID-11633; 0039-9140
- Journal Information:
- Talanta (England), Vol. Vol: 6; Other Information: TID-11633. Orig. Receipt Date: 31-DEC-61
- Country of Publication:
- Country unknown/Code not available
- Language:
- English
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Related Subjects
ACETONE
ALLOYS
AROMATIC HYDROCARBONS
BROMINATED HYDROCARBONS
CERIUM
CERIUM FLUORIDES
CHLORANIL
CHLORANILIC ACID
COBALT
COLOR
DISTILLATION
ELEMENTS
FISSION PRODUCTS
FISSIUM
FUELS
HETEROCYCLICS
HEXANE
HYDROCHLORIC ACID
HYDROFLUORIC ACID
IRON
IRON CHLORIDES
IRON COMPLEXES
ISOMERS
KETONES
LANTHANUM
MANDELIC ACID
MOLYBDENUM
NIOBIUM
ORGANIC ACIDS
ORGANIC NITROGEN COMPOUNDS
PERCHLORIC ACID
PHENANTHROLINE
PHOTOMETRY
PLUTONIUM ALLOYS
PRECIPITATION
QUALITATIVE ANALYSIS
QUANTITATIVE ANALYSIS
QUINONES
REPROCESSING
RUTHENIUM
RUTHENIUM CHLORIDES
SEALS
SOLVENT EXTRACTION
SPECTRA
SULFURIC ACID
TUBES
ZIRCONIUM