This presentation will focus on the use of the Malvern Zetasizer Nano system to characterize novel surfactant systems being developed in our laboratory for DNA separations and gene delivery applications. Because the synthesis of these systems are expensive and fairly low-yield, we needed to identify low-volume, label-free methods to characterize their critical micelle concentrations and size distributions of any structures they formed. The Malvern system is ideally suited for this application. We will discuss some of these results along with tips on obtaining high-quality distributions on low-volume, dilute samples.