Sample preparation for the analysis of nanoparticles in natural waters by single particle ICP-MS

With the significant increase in the production and use of nanoparticles (NP), concern is increasing over their release into their environment. Single particle inductively coupled plasma mass spectrometry (SP-ICP-MS) is emerging as one of the best techniques for detecting the very small NP at very low concentrations in natural waters. However, there is no unified protocol for the preparation of natural water samples for SP-ICP-MS analysis. In order to minimize nebulizer blockage, filtration is often used with the expectation that 0.45 μm membranes will not remove significant quantities of 1-100 nm NP. Nonetheless, there are limited data on its effect on the concentrations or size distributions of the NP. To that end, we examined the interactions between six different membrane filters and silver (Ag) and cerium oxide (CeO₂) NP in aqueous samples. For Ag NP, the highest recoveries were observed for polypropylene membranes, where 55% of the pre-filtration NP were found in rainwater and 75% were found in river waters. For CeO₂ NP, recoveries for the polypropylene membrane attained 60% in rainwater and 75% in river water. Recoveries could be increased to over 80% by pre-conditioning the filtration membranes with a multi-element solution. Similar recoveries were obtained when samples were centrifuged at low centrifugal forces (≤1000×g).