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Application of laser-induced breakdown spectroscopy to assess palladium catalyst deactivation

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Abstract

This work introduces a new method for the investigation of palladium (Pd) catalyst deactivation by laser-induced breakdown spectroscopy (LIBS). For this purpose, deactivation of Pd/(OH)2/C catalyst for synthesis of hexanitrohexaazaisowurtzitane (HNIW or CL-20) as a high-performance energetic compound was studied. The LIBS spectrum of fresh catalyst (Pd/(OH)2/C) with 10% Pd was compared to spent catalyst (Pd/C) containing 7% Pd. LIBS tests were also carried out under argon (Ar) ambient gas in order to correlate with the same tests under air atmosphere. Experimental results indicate that line intensities of Pd were lower for all of the spent catalyst samples under the same conditions. The C2 swan bands are also greater in spent catalyst because of deactivation, which provides a lower amount of Pd in active sites of carbon. Furthermore, the intensity of Hα in spent catalyst is lower than fresh catalyst because of conversion of Pd(OH)2/C to Pd/C during deactivation.

© 2019 Optical Society of America

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