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Determination of trace elements in lithium niobate crystals by solid sampling and solution-based spectrometry

László Bencs1, Krisztina György, Márta Kardos

  • 1Institute for Solid State Physics and Optics, Wigner Research Centre for Physics, Hungarian Academy of Sciences, Budapest, Hungary. bencs.laszlo@wigner.mta.hu

Analytica Chimica Acta
|May 1, 2012
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Summary

This study optimized atomic absorption spectrometry methods for analyzing trace elements like chromium, iron, and manganese in lithium niobate crystals. Solid sampling graphite furnace atomic absorption spectrometry (SS-GFAAS) proved effective for these dopant analyses.

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Area of Science:

  • Analytical Chemistry
  • Materials Science
  • Spectroscopy

Background:

  • Lithium niobate crystals are crucial for optical applications.
  • Accurate determination of dopant elements (Cr, Fe, Mn) is essential for crystal quality.
  • Existing analytical methods may require optimization for direct solid sample analysis.

Purpose of the Study:

  • To develop and optimize analytical methods for trace dopants in lithium niobate.
  • To compare solid sampling (SS) and solution-based (SB) atomic absorption spectrometry techniques.
  • To investigate the chemical forms of the matrix during analysis.

Main Methods:

  • Solid sampling graphite furnace atomic absorption spectrometry (SS-GFAAS).
  • Solution-based methods: GFAAS, flame atomic absorption spectrometry (FAAS), inductively coupled plasma optical emission spectrometry (ICP-OES), and inductively coupled plasma mass spectrometry (ICP-MS).
  • X-ray near-edge absorption structure (XANES) for chemical form analysis.

Main Results:

  • SS-GFAAS calibration achieved using standard addition; SB methods used matrix-matched/acidic standards.
  • Interferences were studied in SB-GFAAS post-digestion.
  • SS-GFAAS required less sensitive lines and higher Ar flow for doped samples.
  • XANES revealed solid matrix vaporizes as metallic form, solution residue as niobium oxide.

Conclusions:

  • SS-GFAAS is a viable method for trace dopant analysis in lithium niobate crystals.
  • Understanding matrix vaporization behavior (metallic vs. oxide) is key for accurate analysis.
  • Method optimization is crucial for handling different sample types and analyte concentrations.