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Title: Spectrophotometric determination of zirconium with xylenol orange

Technical Report ·
DOI:https://doi.org/10.2172/5319653· OSTI ID:5319653

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
Resource Relation:
Other Information: Portions of document are illegible
Country of Publication:
United States
Language:
English