Nanoparticle (NP) characterization is critical in many
fields due
to the use of NPs in numerous applications. Traditional NP characterization
techniques, however, are limited by low sample throughput, and few
can measure the size and elemental composition. Furthermore, sample
throughput limitations are compounded in elemental mapping (EM) techniques
for obtaining NP spatial distribution. Glow discharge optical emission
spectroscopy (GDOES) EM can provide large area maps directly and cost-effectively
from solid samples within tens of seconds. Here, GDOES EM is demonstrated
for the first time for NP characterization in terms of mass, elemental
composition, and size/structure dimensions. The effects of GD pulsed
power, pressure, and sample substrate were studied, and optimized
conditions resulted in limits of detection at single pg levels. While
this is not at the level of single nanoparticle sensitivity, size
differentiation of Ag and Au nanoparticles was successfully demonstrated
between 5 and 100 nm, while the internal dimensions of complex core–shell
NPs were also identified through the optical emission changes as a
function of time.