Spectrophotometric determination of zirconium with xylenol orange
High purity hydride forming metal films are used as hydrogen isotope occluders and function as electrodes in neutron generator tubes. This use of zirconium occluder films requires reliable analytical methods for routine determination of the zirconium film weight in a production environment. In this study, a spectrophotometric method was evaluated for the determination of zirconium films. The method is based upon the formation of a highly colored zirconium complex with xylenol orange in a dilute perchloric acid medium. Dilute hydrofluoric acid is used in this procedure to selectively dissolve the zirconium film off the substrate. A perchloric acid fuming step is used to remove hydrofluoric acid from the solution. The zirconium solutions are depolymerized before complex formation by heating in 2 N perchloric acid. The zirconium complex exhibits a maximum absorbance in 0.2 to 0.3 M perchloric acid at a wavelength of 531 nanometers. Beer's law is obeyed for zirconium concentrations through 2.1 parts per million. Molybdenum, at concentrations equal to zirconium, does not interfere with the xylenol orange method.
- Research Organization:
- General Electric Co., St. Petersburg, FL (USA). Neutron Devices Dept.
- DOE Contract Number:
- AC04-76DP00656
- OSTI ID:
- 5319653
- Report Number(s):
- GEPP-TIS-650; ON: DE82015010
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
400104* -- Spectral Procedures-- (-1987)
ABSORPTION SPECTRA
ACCURACY
CHEMICAL ANALYSIS
COMPLEXES
COMPLEXOMETRY
DATA
DYES
ELECTRODES
ELEMENTS
EXPERIMENTAL DATA
FILMS
HYDROGEN COMPOUNDS
INDICATORS
INFORMATION
INORGANIC ACIDS
METALS
NUMERICAL DATA
PERCHLORIC ACID
QUANTITATIVE CHEMICAL ANALYSIS
RELIABILITY
SPECTRA
SPECTROPHOTOMETRY
TRANSITION ELEMENT COMPLEXES
TRANSITION ELEMENT COMPOUNDS
TRANSITION ELEMENTS
XYLENOL ORANGE
ZIRCONIUM
ZIRCONIUM COMPLEXES
ZIRCONIUM COMPOUNDS