Evaluating the total gold concentration in metallic nanoparticles with a high content of organic matter through microwave-assisted decomposition platform and plasma-based spectrometric techniques (ICP-MS and ICP OES)

We report a complete set of strategies for characterization and an accurate determination of gold in metallic nanoparticles. For this, gold nanorods (AuNR) were synthesized by using the surfactant hexadecyltrimethylammonium bromide (CTAB) as the stabilizer and shape-directing agent. The surfactant CTAB forms a bilayer structure around the nanoparticles and became a challenge for the development of the microwave-assisted decomposition of the AuNR colloid. The bilayer structure of CTAB prevents the Au³⁺ release for the acidic media during the decomposition procedure. To overcome this limitation, a combination of low sample volume consumption (only 200 μL), an acidic mixture of reverse aqua regia (1:3 v/v, HCl:HNO₃), and sulfuric acid, and a microwave program was used. The gold quantification by ICP-MS and checked through the ICP OES, demonstrated that the seed-mediated growth method used for the AuNR synthesis has a high yield, presenting ca. 100% of gold content (ca. 100 mg L⁻¹ of gold concentration) in the post-synthesis colloid (AuNR-total) as well as in the colloid after a washing step (AuNR-res). The microwave-assisted decomposition procedure also demonstrated to be efficient in the acidic decomposition of the gold-silver core-shell nanoparticle (Au@AgNR), which presents a high content of polyvinylpyrrolidone (PVP) (Mw ~55000 g mol⁻¹) acting as a stabilizer, in addition to the matrix with CTAB. The results demonstrated an accurate recovery of ca. 100% of gold content for the Au@AgNR regarding the gold nanorod before the growth of the silver shell (AuNR_Core). The proposed microwave-assisted decomposition platform demonstrated to be an efficient, reliable, and robust characterization tool for the gold quantification in metallic nanoparticles, presenting no interference of the complex matrix with high organic content.