High-Quality In Situ X-ray Absorption Spectroscopy Monitoring of the Palladium Nucleation inside the 3D Printed Microfluidic Chip

An efficient approach for high-quality X-ray absorption spectroscopy (XAS) measurements is proposed and exemplified by monitoring the nucleation of palladium nanoparticles from Pd(II) acetate. The idea of an X-ray beam passing through a microfluidic channel allowed for a significant improvement of the data quality to monitor in situ the early stages of palladium nanoparticle formation. The time evolution of Pd(II) and Pd(0) fractions was followed by collecting the spectra in seven subsequent channels and quantified by linear combination analysis of Pd foil and Pd acetate reference spectra. This work illustrates the application of XAS in microfluidics for chemical systems and might be used for obtaining structural information under reaction conditions in the presence of 4d metals.

Automated summary

An efficient approach using X-ray absorption spectroscopy (XAS) was proposed to monitor the nucleation of palladium nanoparticles from Pd(II) acetate. By passing an X-ray beam through a microfluidic channel, the data quality was significantly improved for in situ monitoring of the early stages of nanoparticle formation. The time evolution of Pd(II) and Pd(0) fractions was quantified using linear combination analysis of Pd foil and Pd acetate reference spectra. This work demonstrates the application of XAS in microfluidics for studying chemical systems and obtaining structural information under reaction conditions with 4d metals.