Standardization of microwave-assisted extraction procedures for characterizing non-labile metallic nanoparticles in environmental solid samples by means of single particle ICP-MS

Abstract

Microwave-assisted extraction (MAE) treatments seem to be a promising sample preparation strategy to isolate nanomaterials (NMs) from environmental samples prior to single particle inductively coupled plasma mass (spICP-MS) determination. Nevertheless, because previous studies make use of domestic microwave ovens (DMOs), several shortcomings arise that compromise the analysis such as lack of control of experimental variables, limited operating conditions, and uncontrolled sample heating leading to irreproducibility issues. The goal of this work is to adapt previously developed MAE treatments for soil and air filters with the DMO apparatus to state-of-the-art scientific microwave ovens (SMOs) in order to standardize current analytical protocols for NM characterization. Results show that, by working with an SMO, non-labile metallic NMs (Pt-AuNPs) are quantitively extracted from soil and air filter samples unaltered in 10 min and 6 min, respectively, at 1200 W by using 10 mL of NaOH 0.1 M solution. The use of a SMO system allows improving accuracy (above 10% of the particle recovery), precision (above 5% of the RSD) and sample throughput (above 4-fold) when compared to the DMO ones. According to these findings, MAE seems to be a powerful strategy for routine analysis of non-labile NMs in environmental samples.