Direct non-destructive total reflection X-ray fluorescence elemental determinations in zirconium alloy samples

Area of Science:

• Materials Science
• Analytical Chemistry
• Nuclear Engineering

Background:

• Traditional elemental analysis of metal alloys often requires sample dissolution and matrix separation.
• Zirconium alloys are critical materials, particularly in the nuclear industry, necessitating precise elemental characterization.
• Existing methods for zirconium alloy analysis can be destructive and generate significant analytical waste.

Purpose of the Study:

• To develop and validate a direct, non-destructive analytical methodology for elemental determination in zirconium alloys using synchrotron-radiation-based total reflection X-ray fluorescence (TXRF).
• To establish a method capable of quantifying multiple elements with high precision and accuracy in zirconium alloy samples.
• To provide an alternative to traditional destructive analytical techniques, reducing sample preparation complexity and waste generation.

Main Methods:

• Development of a direct total reflection X-ray fluorescence (TXRF) analytical methodology utilizing synchrotron radiation.
• Sample preparation involved mirror polishing of zirconium alloy discs (Zr-2.5%Nb and Zircalloy-4) without dissolution.
• TXRF measurements were performed at two excitation energies (1.9 keV and 14 keV) using two quantification schemes (fundamental parameter and relative sensitivity based methods).
• Validation of TXRF results through comparison with DC arc carrier distillation atomic emission spectrometry.

Main Results:

• Successful development of a direct, non-destructive TXRF methodology for elemental analysis of zirconium alloys.
• Quantification of fifteen minor and trace elements with high precision and accuracy relative to Zr.
• Excellent agreement between TXRF results and those obtained from DC arc carrier distillation atomic emission spectrometry.
• Demonstration of the method's capability to analyze samples directly after polishing and cleaning, avoiding dissolution.

Conclusions:

• The developed synchrotron-radiation-based TXRF methodology offers a direct, non-destructive, precise, and accurate approach for elemental characterization of zirconium alloys.
• This method significantly simplifies sample preparation, eliminates the need for dissolution and matrix separation, and substantially reduces analytical waste.
• The methodology is suitable for various industrial applications beyond the nuclear industry, offering a versatile analytical solution.