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.