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Updated: May 19, 2026
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
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.
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.
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