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Atomic Emission Spectroscopy: Overview01:20

Atomic Emission Spectroscopy: Overview

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Confocal micro-x-ray fluorescence spectrometer for light element analysis.

S Smolek1, B Pemmer, M Fölser

  • 1Atominstitut, Vienna University of Technology, Stadionallee 2, 1020 Vienna, Austria. smolek@ati.ac.at

The Review of Scientific Instruments
|September 4, 2012
PubMed
Summary
This summary is machine-generated.

This study introduces a confocal micro-XRF spectrometer for 3D elemental analysis. The enhanced system achieves micrometer resolution and ppm detection limits for light elements.

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Area of Science:

  • Materials Science
  • Analytical Chemistry
  • Spectroscopy

Background:

  • Micro-X-ray fluorescence (micro-XRF) is a powerful technique for elemental analysis.
  • Existing micro-XRF spectrometers are typically limited to 2D analysis.
  • Light element analysis (6 ≤ Z ≤ 14) presents unique challenges.

Purpose of the Study:

  • To upgrade an existing micro-XRF spectrometer for true 3D elemental analysis.
  • To enhance the spatial resolution and detection capabilities of the instrument.
  • To characterize the performance of the confocal micro-XRF system.

Main Methods:

  • Modified an existing micro-XRF spectrometer by adding a second polycapillary x-ray optic and piezo positioners.
  • Operated the spectrometer in a confocal geometry within a vacuum chamber.
  • Utilized two x-ray tubes (Mo and Rh anodes) for excitation.
  • Determined depth resolution and lower limits of detection (LLD).
  • Compared results with synchrotron radiation (SR) micro-XRF.

Main Results:

  • Achieved true 3D elemental analysis in the micrometer regime.
  • Depth resolution ranged from 100 microm (Na-Kα) to 30 microm (Mo).
  • Lower limits of detection were in the parts-per-million (ppm) range.
  • The system demonstrated capabilities and limitations when compared to SR micro-XRF.

Conclusions:

  • The confocal micro-XRF spectrometer enables 3D elemental mapping with micrometer resolution.
  • The upgraded system significantly enhances analytical capabilities for light elements.
  • Further characterization and comparison with SR micro-XRF provide insights into its performance and applications.