Determination of Size, Size Distribution, and Concentration of Nanoparticles Using ICP‐MS in the Context of SERS Substrates

ABSTRACT Surface enhanced Raman scattering (SERS) is a widely used vibrational spectroscopic technique employing metallic nanostructures to enhance an inherent Raman signal. This study aimed to develop a method for the characterization of SERS substrates in a single analysis by inductively coupled plasma mass spectrometry (ICP‐MS) equipped with the single particle module (spICP‐MS). For this development, the well‐known Lee‐Meisel protocol was selected as starting point to synthesize gold nanoparticles (AuNps) and silver nanoparticles (AgNps). A spICP‐MS method was successfully developed and gave the mean size, size distribution, and concentration of nanoparticles in only one single analysis. Reference techniques were used to confirm these results namely dynamic light scattering, transmission electron microscopy, and UV–Visible spectroscopy. Thanks to the ICP‐MS characterization, it was observed that AgNps synthesized by chemical reduction presented more variability than the AuNps. The dissolved elements concentration in the suspension was investigated. It appeared that reaction yields were close to 100% for the six syntheses. This analysis may be repeated over time to evaluate the suspension stability and monitor any potential degradation of Nps. To conclude, ICP‐MS is a powerful technique to characterize SERS substrates and could be an interesting alternative to other characterization techniques.