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Related Experiment Video

Updated: May 19, 2026

The Synthesis, Characterization and Reactivity of a Series of Ruthenium N-triphosPh Complexes
10:51

The Synthesis, Characterization and Reactivity of a Series of Ruthenium N-triphosPh Complexes

Published on: April 10, 2015

Ruthenium Speciation during Acidification of Alkaline Solution.

Mathis Leblanc1, Sarah Baghdadi1, Philippe M Martin1

  • 1CEA, DES, ISEC, DMRC, Univ Montpellier, 30207 Marcoule, France.

ACS Omega
|May 18, 2026
PubMed
Summary

Ruthenium analysis is hindered by precipitation during acidification. This study monitored ruthenium speciation in real-time, revealing a two-step mechanism and an amorphous precipitate, crucial for accurate ICP-MS measurements.

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Area of Science:

  • Analytical Chemistry
  • Nuclear Chemistry
  • Materials Science

Background:

  • Ruthenium (Ru) is a volatile fission product with nuclear medicine applications.
  • Alkaline gas traps capture volatile ruthenium, but subsequent acidification for analysis (ICP-MS/ICP-OES) causes precipitation, leading to inaccurate results.
  • Accurate ruthenium determination is critical, yet sample preparation challenges persist.

Purpose of the Study:

  • To monitor ruthenium speciation during the acidification of alkaline solutions with nitric acid.
  • To elucidate the reaction mechanism and identify precipitated species.
  • To develop a method for accurate ruthenium analysis in alkaline samples.

Main Methods:

  • Real-time monitoring of ruthenium speciation using a closed reactor coupled with in situ high-speed UV-visible spectroscopy.
  • Quantitative recovery of gaseous and solid byproducts to close the analytical mass balance.
  • Characterization of the precipitate using thermogravimetric analysis (TGA), X-ray diffraction (XRD), Raman spectroscopy, and X-ray absorption near-edge structure (XANES).

Main Results:

  • A two-step reaction mechanism was identified, involving soluble species formation, ruthenium tetroxide (RuO4) volatilization, and amorphous phase precipitation.
  • Structural analyses confirmed the precipitate's unique nature, distinct from known ruthenium oxides or ruthenates.
  • XANES indicated the presence of Ru(+V) and limited stability of the species under experimental conditions.

Conclusions:

  • The study provides a detailed methodology for monitoring ruthenium speciation during nitric acid acidification.
  • Proposed reaction pathways involve ruthenate and perruthenate intermediates forming RuO4 and Ru2O5.
  • This research addresses a critical gap in ICP-MS sample preparation for alkaline ruthenium solutions.