BARC/PUB/2004/0383

 
 

Determination of elemental composition of Zr-Nb alloys by Glow Discharge Quadrupole Mass Spectrometry

 
     
 
Author(s)

Shekhar, R.; Arunachalam, J.; Radha Krishna, G.; and others
(CCCM)

Source

Atomic Spectroscopy, 2004. Vol. 25 (4): pp. 157-164

ABSTRACT

The simultaneous determination of trace elements and niobium in Zr-Nb alloys with varying niobium concentrations has been carried out by Glow Discharge Quadrupole Mass Spectrometry (GD-QMS). The Relative Sensitivity Factors (RSF) for the analytes were generated using a certified reference material of a zirconium alloy (zircaloy, non-similar matrix composition). GD-QMS results have been found to be in good agreement with the certified concentrations for several elements of other zirconium-based certified reference materials (zirco-nium metal and alloys).

     This technique is a viable alternative to validate  conventional atomic emission and other spectrometric techniques used for the determination of impurities in zirconium-based alloys. With the optimized discharge conditions and pre-sputtering time, the precision of measurements achieved were typically 1% RSD for the majority of elements present at mg kg –1 levels, 10% RSD for μg kg –1 levels, 0.05% RSD for zirconium (matrix), and  0.05% RSD for niobium (alloying element).

     The detection limits for the analytes were found to be at sub - ppm levels with an integration time of 20ms, 140 points, and four repetitive scans. Molecular interferences observed due to oxygen, matrix, and argon are also listed.

 
 
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